Preparation method of organic silicon hybridized acrylate pressure-sensitive glue and pressure-sensitive adhesive tape

By copolymerizing (meth)acrylate silicone monomers with acrylate monomers and crosslinking agents, the adhesive layer achieves enhanced wettability and adhesion to silicon-based materials, addressing poor adhesion and water seepage issues in existing tapes.

CN119242223APending Publication Date: 2025-01-03ZHEJIANG SUNLIKY NEW MATERIAL TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411367071.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-29
Publication Date
2025-01-03

AI Technical Summary

Technical Problem

Existing acrylic pressure-sensitive tapes exhibit poor wettability and adhesion to silicon-based materials, leading to bubble formation and water seepage during cleaning, which affects the quality of high-end manufacturing processes.

Method used

A method involving copolymerization of (meth)acrylate silicone monomers with acrylate soft, hard, and functional monomers, along with silicone crosslinking agents and additives, to create a silicone hybrid acrylate pressure-sensitive adhesive with reduced surface energy and improved flexibility, enhancing adhesion to silicon-based substrates.

Benefits of technology

The adhesive layer demonstrates improved wettability and viscosity, preventing bubble formation and water seepage, ensuring better adhesion and quality control in high-end manufacturing processes.

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Abstract

The invention provides a preparation method of organic silicon hybridized acrylate pressure-sensitive glue and a pressure-sensitive adhesive tape, and relates to the technical field of adhesives. (methyl) acrylate organic silicon monomers with higher copolymerization reaction activity with acrylate and other (methyl) acrylate soft monomers, hard monomers, functional monomers and the like are subjected to copolymerization reaction; introducing a monomer containing an organic silicon side chain to a polymer main chain to obtain an organic silicon hybridized acrylate main glue solution; and mixing the organic silicon hybridized acrylate main glue solution with an organic silicon flexible cross-linking agent, a tackifier, an antioxidant and other additives to obtain the organic silicon hybridized acrylate pressure-sensitive glue. The main component of the adhesive layer of the pressure-sensitive adhesive tape prepared from the organosilicone hybridized acrylate pressure-sensitive adhesive is an acrylate polymer into which a large proportion of organosilicone groups are introduced, so that the wettability of the adhesive layer of the pressure-sensitive adhesive tape to a silicon-based substrate is better, and the adhesion of the adhesive tape to the substrate is improved.
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Description

Technical Field

[0001] The invention relates to the technical field of adhesives, and in particular to a method for preparing a silicone hybrid acrylate pressure-sensitive adhesive and a pressure-sensitive adhesive tape. Background Art

[0002] In the fields of integrated circuits, microprocessor manufacturing, high-frequency electronic devices and new energy, high-purity silicon, single crystal silicon, silicon dioxide, silicon carbide, silicon nitride and the like are widely used as base materials. Without surface treatment, the surface energy of such silicon-based materials is low, and the common chemical systems of glues such as acrylates and polyurethanes have strong polarity and poor wettability to silicon-based materials. Therefore, after the acrylic pressure-sensitive tape is attached to the silicon substrate, bubbles or gaps are likely to appear at the interface between the tape adhesive layer and the silicon substrate, which not only affects the appearance, but also has poor attachment effect. Water seepage is likely to occur during the product cleaning and washing process, which has a huge impact on the quality control of high-end manufacturing. Therefore, while ensuring that the adhesive layer of the acrylic pressure-sensitive tape has high viscosity, how to further improve the wettability of the adhesive layer of the acrylic pressure-sensitive tape to silicon-based materials has become a problem that needs to be solved urgently. Summary of the invention

[0003] The problem solved by the present invention is: how to further improve the wettability of the adhesive layer of the acrylic pressure-sensitive adhesive tape to the silicon-based material while ensuring that the adhesive layer of the acrylic pressure-sensitive adhesive tape has high viscosity.

[0004] In order to solve the above problems, the present invention provides a method for preparing a silicone hybrid acrylate pressure-sensitive adhesive, comprising:

[0005] Step S1: Under an inert gas protection atmosphere, copolymerizing the first mixture to obtain a silicone hybrid acrylate main glue solution; wherein, the first mixture comprises, by weight: 20-90 parts of soft monomers, 0.5-40 parts of hard monomers, 0.5-20 parts of functional monomers, 0.5-20 parts of (meth)acrylate silicone monomers, 0.5-1 parts of thermal initiators and 50-200 parts of organic solvents;

[0006] Step S2: adding the second mixture to the organosilicon-hybridized acrylate main adhesive solution and mixing them evenly to obtain the organosilicon-hybridized acrylate pressure-sensitive adhesive; wherein the second mixture comprises, by weight, 1-50 parts of a tackifier and 1-10 parts of an antioxidant.

[0007] Optionally, in step S1, the (meth)acrylate silicone monomer includes at least one of 3-(trimethoxysilyl)propyl acrylate, 3-(methoxydimethylsilyl)propyl acrylate, 3-[diethoxy(methyl)silyl]propyl methacrylate, 3-(methacryloyloxy)propyltrimethoxysilane, 3-methacryloyloxypropylmethyldimethoxysilane and 3-(methacryloyloxy)propyltriethoxysilane.

[0008] Optionally, in step S1, the first mixture further comprises 0.1-10 parts of an internal crosslinking agent, wherein the internal crosslinking agent comprises one of 1,3-bis(3-methacryloxypropyl)tetrakis(trimethylsiloxy)disiloxane and a polysiloxane compound having a plurality of (meth)acrylic functional end groups with double bonds.

[0009] Optionally, in step S2, the second mixture further comprises 0.1-10 parts of an external crosslinking agent, and the external crosslinking agent comprises one of an epoxy-terminated polysiloxane compound, a multifunctional isocyanate, a multifunctional aziridine, a high-valent metal acid ester and a metal chelate.

[0010] Optionally, in step S1, the soft monomer includes at least one of (meth) alkyl acrylates with a branched or linear structure between C7 and C15; the hard monomer includes at least one of methyl methacrylate, ethyl acrylate and isobornyl acrylate; the functional monomer includes at least one of acrylic acid, acrylamide and 2-aminoethyl methacrylate hydrochloride; the thermal initiator includes at least one of azobisisobutyronitrile, azobisisovaleronitrile, azobisisoheptylonitrile and dibenzoyl peroxide; and the organic solvent includes at least one of ethyl acetate, butyl acetate, acetone, methyl ethyl ketone, benzene and toluene.

[0011] Optionally, in step S2, the antioxidant includes at least one of a phenolic antioxidant, an amine antioxidant and a phosphite antioxidant, and the tackifier includes at least one of a rosin resin, a hydrocarbon and a terpene resin.

[0012] Optionally, in step S1, the copolymerization reaction temperature is 60-90° C. and the reaction time is 8-14 h.

[0013] The present invention also provides a method for preparing a pressure-sensitive adhesive tape, comprising:

[0014] Step M1: coating the organosilicon hybrid acrylate pressure-sensitive adhesive on the base film and drying it to obtain a pressure-sensitive adhesive layer; the organosilicon hybrid acrylate pressure-sensitive adhesive is prepared by the preparation method of the organosilicon hybrid acrylate pressure-sensitive adhesive;

[0015] Step M2: A release film is attached to the surface of the pressure-sensitive adhesive layer to obtain a pressure-sensitive adhesive tape.

[0016] Optionally, in step M1, the thickness of the base film is 50-200 μm, and the thickness of the pressure-sensitive adhesive layer is 5-50 μm.

[0017] Optionally, in step M1, the material of the base film is selected from one of polypropylene, polyethylene, polyolefin, polyethylene terephthalate and polyvinyl chloride.

[0018] Compared with the prior art, the present invention uses (meth) acrylate silicone monomers with high copolymerization activity with acrylate to copolymerize with acrylate soft monomers, hard monomers, functional monomers, etc., and introduces monomers containing silicone side chains on the main chain of the polymer to obtain silicone hybrid acrylate main glue solution; then the silicone hybrid acrylate main glue solution is mixed with a flexible silicone crosslinking agent, a tackifier, and an antioxidant to obtain silicone hybrid acrylate pressure-sensitive adhesive. The silicone group has a lower intermolecular force and higher flexibility. In the process of preparing the pressure-sensitive tape, the present invention simultaneously introduces a larger proportion of silicone groups in the two steps of copolymerization and crosslinking, so that the surface energy of the adhesive layer of the pressure-sensitive tape is significantly reduced, which can effectively improve the wettability of the adhesive layer of the pressure-sensitive tape to the silicon-based substrate. In addition, it has been tested that the adhesive layer of the pressure-sensitive tape prepared by the present invention also has a higher viscosity. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 The figure is a schematic diagram of the preparation method of the organosilicon hybrid acrylate pressure-sensitive adhesive in the embodiment of the present invention;

[0020] Figure 2 Schematic diagram of the structure of the pressure-sensitive adhesive tape in an embodiment of the present invention.

[0021] Description of reference numerals:

[0022] 1. Base film; 2. Pressure-sensitive adhesive layer; 3. Release film. DETAILED DESCRIPTION

[0023] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below in conjunction with the accompanying drawings. Although certain embodiments of the present invention are shown in the accompanying drawings, it should be understood that the present invention can be implemented in various forms and should not be interpreted as being limited to the embodiments described herein. On the contrary, these embodiments are provided to provide a more thorough and complete understanding of the present invention. It should be understood that the drawings and embodiments of the present invention are only for exemplary purposes and are not intended to limit the scope of protection of the present invention.

[0024] Unless otherwise defined, all technical and scientific terms used in this application have the same meanings as those commonly understood by those skilled in the art to which this application belongs; the terms used in the specification of this application are only for the purpose of describing specific implementation methods and are not intended to limit this application;

[0025] The term "including" and its variations used in this article are open inclusions, that is, "including but not limited to"; the term "based on" is "based at least in part on"; the term "one embodiment" means "at least one embodiment"; the term "another embodiment" means "at least one other embodiment"; the term "some embodiments" means "at least some embodiments"; the term "optionally" means "optional embodiments". The relevant definitions of other terms will be given in the following description. It should be noted that the concepts of "first" and "second" mentioned in the present invention are used to distinguish different objects, rather than to describe a specific order or a primary and secondary relationship. In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of this application, unless otherwise specified, the meaning of "multiple" is two or more.

[0026] like Figure 1 As shown, a method for preparing a silicone hybrid acrylate pressure-sensitive adhesive provided by an embodiment of the present invention comprises:

[0027] Step S1: Under an inert gas protection atmosphere, copolymerizing the first mixture to obtain a silicone hybrid acrylate master glue solution; wherein, the first mixture comprises, by weight: 20-90 parts of soft monomers, 0.5-40 parts of hard monomers, 0.5-20 parts of functional monomers, 0.5-20 parts of (meth)acrylate silicone monomers, 0.5-1 parts of thermal initiators and 50-200 parts of organic solvents; preferably, by weight, the first mixture comprises: 50-80 parts of soft monomers, 3-20 parts of hard monomers, 1-15 parts of functional monomers, 2-10 parts of (meth)acrylate silicone monomers, 0.5-1 parts of thermal initiators and 50-200 parts of organic solvents;

[0028] Step S2: adding the second mixture to the organosilicon-hybridized acrylate main adhesive solution and mixing them evenly to obtain the organosilicon-hybridized acrylate pressure-sensitive adhesive; wherein the second mixture comprises, by weight, 1-50 parts of a tackifier and 1-10 parts of an antioxidant.

[0029] The embodiment of the present invention uses (meth)acrylate silicone monomers with high copolymerization activity with acrylate to copolymerize with acrylate soft monomers, hard monomers, functional monomers, etc., and introduces monomers containing silicone side chains on the main chain of the polymer to obtain silicone hybrid acrylate main glue solution; then the silicone hybrid acrylate main glue solution is mixed with a tackifier, an antioxidant, etc. to obtain silicone hybrid acrylate pressure-sensitive adhesive. The silicone group has a lower intermolecular force and higher flexibility. In the process of preparing the pressure-sensitive tape in the embodiment of the present invention, a larger proportion of silicone groups is introduced in the copolymerization step, so that the surface energy of the adhesive layer of the pressure-sensitive tape is significantly reduced, which can effectively improve the wettability of the adhesive layer of the pressure-sensitive tape to the silicon-based substrate. In addition, it has been tested that the adhesive layer of the pressure-sensitive tape prepared in the embodiment of the present invention also has a higher viscosity.

[0030] In some embodiments of the present invention, in step S1, the first mixture further includes 0.1-10 parts of an internal crosslinking agent, preferably, the first mixture further includes 0.2-5 parts of an internal crosslinking agent; the internal crosslinking agent includes one of 1,3-bis(3-methacryloxypropyl)tetra(trimethylsiloxy)disiloxane and a polysiloxane compound having multiple (meth)acrylic functional end groups with double bonds. Exemplarily, the polysiloxane compound having multiple (meth)acrylic functional end groups with double bonds is a methacryloxypropyl double-terminated polydimethylsiloxane or a (3-acryloxy-2-hydroxypropoxypropyl)-terminated polydimethylsiloxane. Due to the difference in reactivity, the use of (meth)acrylate organosilicon monomers for copolymerization will lead to the problem of insufficient monomer conversion rate, thereby limiting the introduction ratio of organosilicon groups in the main component acrylate polymer of the pressure-sensitive tape adhesive layer and making the ratio of added copolymer monomers too different from the actual monomers of the polymer. In this embodiment, since an internal cross-linking agent is added to the first mixture, the internal cross-linking agent participates in the cross-linking reaction during the copolymerization reaction, and the organosilicon groups on the side chains do not participate in the reaction, so more organosilicon groups can be introduced into the main chain of the acrylate polymer (the main component of the adhesive layer of the pressure-sensitive tape), which is beneficial to further improve the wetting effect of the adhesive layer of the pressure-sensitive tape on the silicon-based substrate.

[0031] In some embodiments of the present invention, in step S2, the second mixture further includes 0.1-10 parts of an external crosslinking agent, and preferably, the second mixture further includes 0.5-10 parts of an external crosslinking agent. The external crosslinking agent includes one of an epoxy-terminated polysiloxane compound, a multifunctional isocyanate, a multifunctional aziridine, a high-valent metal acid ester, and a metal chelate; illustratively, the epoxy-terminated polysiloxane compound is 1,3-bis(3-glycidyloxypropyl)-1,1,3,3-tetramethyldisiloxane. Due to the difference in reactivity, the use of (meth)acrylate silicone monomers for copolymerization will lead to the problem of insufficient monomer conversion rate, thereby limiting the introduction ratio of silicone groups in the main component acrylate polymer of the pressure-sensitive tape adhesive layer and the difference between the proportion of added copolymer monomers and the actual monomers of the polymer is too large. When the external cross-linking agent is an epoxy-terminated polysiloxane compound, since a flexible silicone external cross-linking agent is added to the second mixture, in the subsequent curing process, the carboxyl group, amine group, etc. on the polymer main chain generated by the previous copolymerization reaction can undergo a cross-linking reaction with the external cross-linking agent, and more silicone groups can be introduced into the acrylate polymer (the main component of the adhesive layer of the pressure-sensitive tape), which is beneficial to further improve the wetting effect of the adhesive layer of the pressure-sensitive tape on the silicon-based substrate.

[0032] In some embodiments of the present invention, in step S1, the (meth)acrylate silicone monomer includes at least one of 3-(trimethoxysilyl)propyl acrylate, 3-(methoxydimethylsilyl)propyl acrylate, 3-[diethoxy(methyl)silyl]propyl methacrylate, 3-(methacryloyloxy)propyltrimethoxysilane, 3-methacryloyloxypropylmethyldimethoxysilane and 3-(methacryloyloxy)propyltriethoxysilane.

[0033] In some embodiments of the present invention, in step S1, the soft monomer includes at least one of (meth) alkyl acrylates with a branched or linear structure between C7 and C15; for example, the soft monomer includes at least one of butyl acrylate (BA), amyl acrylate, hexyl acrylate, heptyl acrylate, hexylethyl acrylate (EHA) and isooctyl acrylate; the hard monomer includes at least one of methyl methacrylate (MMA), ethyl acrylate (EA) and isobornyl acrylate (IBOA); the functional monomer includes at least one of acrylic acid (AA), acrylamide (ACM) and 2-aminoethyl methacrylate hydrochloride; the thermal initiator includes at least one of azobisisobutyronitrile (AIBN), azobisisovaleronitrile, azobisisoheptonitrile and dibenzoyl peroxide; the organic solvent includes at least one of ethyl acetate, butyl acetate, acetone, methyl ethyl ketone, benzene and toluene.

[0034] In some embodiments of the present invention, in step S2, the antioxidant includes at least one of a phenolic antioxidant, an amine antioxidant and a phosphite antioxidant, such as the antioxidant Irganox 1010, and the tackifier includes at least one of a rosin resin, a hydrocarbon and a terpene resin, such as the tackifier EASTMAN 168.

[0035] In some embodiments of the present invention, in step S1, the copolymerization reaction temperature is 60-90° C. and the time is 8-14 h.

[0036] The embodiment of the present invention also provides a method for preparing a pressure-sensitive adhesive tape, comprising:

[0037] Step M1: coating the organosilicon hybrid acrylate pressure-sensitive adhesive on the base film 1 and drying it to obtain a pressure-sensitive adhesive layer 2; the organosilicon hybrid acrylate pressure-sensitive adhesive is prepared by the preparation method of the organosilicon hybrid acrylate pressure-sensitive adhesive;

[0038] Step M2: Paste the release film 3 on the surface of the pressure-sensitive adhesive layer 2 to obtain a pressure-sensitive adhesive tape, such as Figure 2 shown.

[0039] In some embodiments of the present invention, in step M1, the thickness of the base film 1 is 50-200 μm, preferably 50-150 μm, and the thickness of the pressure-sensitive adhesive layer 2 is 5-50 μm, preferably 5-20 μm.

[0040] In some embodiments of the present invention, in step M1, the material of the base film 1 is selected from one of polypropylene, polyethylene, polyolefin, polyethylene terephthalate and polyvinyl chloride.

[0041] In some embodiments of the present invention, in step M1, the drying temperature is 60° C. and the drying time is 24 hours.

[0042] The present invention is further described below in conjunction with specific embodiments.

[0043] Example 1

[0044] A1: Under an inert gas protection atmosphere, the first mixture is subjected to a copolymerization reaction to obtain a silicone hybrid acrylate main glue solution; wherein the first mixture consists of 75 grams of EHA, 15 grams of MMA, 5 grams of AA, 5 grams of 3-(trimethoxysilyl)propyl acrylate, 0.5 grams of azobisisobutyronitrile and 100 grams of ethyl acetate; wherein the copolymerization temperature is 80°C and the time is 12 hours.

[0045] A2: Add the second mixture to the silicone hybrid acrylate main adhesive solution and mix them evenly to obtain a silicone hybrid acrylate pressure-sensitive adhesive; wherein the second mixture consists of 5 grams of tackifier EASTMAN 168, 2 grams of external cross-linking agent and 1 gram of antioxidant Irganox 1010; wherein the external cross-linking agent is 1,3-bis(3-glycidyloxypropyl)-1,1,3,3-tetramethyldisiloxane.

[0046] A3: The silicone hybrid acrylate pressure-sensitive adhesive is coated on the polyolefin base film and dried to obtain a pressure-sensitive adhesive layer; the drying temperature is 60°C and the time is 24 hours; the thickness of the polyolefin base film is 100 μm, and the thickness of the pressure-sensitive adhesive layer is 10 μm.

[0047] A4: A release film is attached to the surface of the pressure-sensitive adhesive layer to obtain a pressure-sensitive adhesive tape.

[0048] Example 2

[0049] The difference from Example 1 is that in step A1, the first mixture consists of 75 g of EHA, 15 g of MMA, 5 g of AA, 5 g of 3-(trimethoxysilyl)propyl acrylate, 0.5 g of azobisisobutyronitrile, 2 g of an internal cross-linking agent and 100 g of ethyl acetate; wherein the internal cross-linking agent is (3-acryloxy-2-hydroxypropoxypropyl) end-capped polydimethylsiloxane; in step A2, the second mixture consists of 5 g of tackifier EASTMAN 168 and 1 g of antioxidant Irganox 1010.

[0050] Example 3

[0051] The difference from Example 1 is that in step A1, the first mixture consists of 60 g EHA, 15 g MMA, 5 g 2-aminoethyl methacrylate hydrochloride, 5 g 3-(trimethoxysilyl)propyl acrylate, 0.5 g azobisisobutyronitrile and 100 g ethyl acetate.

[0052] Example 4

[0053] The difference from Example 1 is that in step A1, the first mixture consists of 60 grams of EHA, 15 grams of MMA, 5 grams of 2-aminoethyl methacrylate hydrochloride, 5 grams of 3-(trimethoxysilyl)propyl acrylate, 0.5 grams of azobisisobutyronitrile, 2 grams of an internal cross-linking agent and 100 grams of ethyl acetate; wherein the internal cross-linking agent is (3-acryloxy-2-hydroxypropoxypropyl) end-capped polydimethylsiloxane.

[0054] Example 5

[0055] The difference from Example 1 is that in step A2, the second mixture consists of 5 grams of tackifier EASTMAN 168, 1 gram of antioxidant Irganox 1010 and 2 grams of aluminum acetylacetonate.

[0056] Comparative Example 1

[0057] The difference from Example 1 is that in step A1, the first mixture consists of 80 g of EHA, 15 g of MMA, 5 g of AA, 0.5 g of azobisisobutyronitrile and 100 g of ethyl acetate; in step A2, the second mixture consists of 5 g of tackifier EASTMAN168, 1 g of antioxidant Irganox 1010 and 2 g of external cross-linking agent, and the external cross-linking agent is aluminum acetylacetonate.

[0058] Comparative Example 2

[0059] The difference from Example 1 is that in step A1, the first mixture consists of 80 g of EHA, 15 g of MMA, 5 g of AA, 0.5 g of azobisisobutyronitrile and 100 g of ethyl acetate.

[0060] Comparative Example 3

[0061] The difference from Example 2 is that in step A1, the first mixture consists of 80 g EHA, 15 g MMA, 5 g AA, 2 g internal crosslinking agent, 0.5 g azobisisobutyronitrile and 100 g ethyl acetate; wherein the internal crosslinking agent is 1,6-hexanediol diacrylate.

[0062] Comparative Example 4

[0063] The difference from Example 2 is that in step A1, the first mixture consists of 80 grams of EHA, 15 grams of MMA, 5 grams of AA, 2 grams of internal cross-linking agent, 0.5 grams of azobisisobutyronitrile and 100 grams of ethyl acetate; wherein the internal cross-linking agent is (3-acryloxy-2-hydroxypropoxypropyl) end-capped polydimethylsiloxane.

[0064] Test results analysis

[0065] The 180° peeling force, water drop contact angle, silicon-based wafer wetting time, and water seepage during silicon-based wafer cutting of the pressure-sensitive adhesive tapes prepared in Examples 1-5 and Comparative Examples 1-4 were tested, and the results are shown in Table 1. As can be seen from Table 1, the pressure-sensitive adhesive tapes prepared in Examples 1-5 and Comparative Examples 1-4 all have a high 180° peeling force (above 8.0N / 25mm) and high viscosity. Compared with Comparative Examples 1-4, the water drop contact angle of the pressure-sensitive adhesive tape prepared in Examples 1-5 is larger, indicating that the adhesive layer of the pressure-sensitive adhesive tape prepared in Examples 1-5 has a lower surface energy and can better wet the silicon-based material with lower surface energy. Compared with Comparative Examples 1-4, the silicon-based wafer wetting time of the pressure-sensitive adhesive tape prepared in Examples 1-5 is shorter, which proves that the pressure-sensitive adhesive tape prepared in Examples 1-5 can better wet the silicon-based material. The pressure-sensitive adhesive tapes prepared in Comparative Examples 1-4 had water seepage during wafer dicing, while the pressure-sensitive adhesive tapes prepared in Examples 1-5 did not have water seepage during wafer dicing, indicating that the pressure-sensitive adhesive tapes prepared in Examples 1-5 had better adhesion to the silicon-based substrate, further confirming that the pressure-sensitive adhesive tapes prepared in Examples 1-5 could better wet the silicon-based material. Compared with Example 5, the water drop contact angle of the pressure-sensitive adhesive tapes prepared in Examples 1-4 was larger, and the silicon-based wafer wetting time was shorter, indicating that the pressure-sensitive adhesive tapes prepared in Examples 1-4 could better wet the silicon-based material.

[0066] Table 1

[0067]

[0068] The adhesive tape performance testing method involved in the present invention is as follows:

[0069] 1) 180° peel strength test of adhesive tape: carried out in accordance with GB / T2792-2014 standard.

[0070] 2) Water drop contact angle test: Use the sessile drop method to test the water drop contact angle of different adhesive surfaces, that is, drop ultrapure water directly on the tape surface, and then use an optical microscope or a dedicated contact angle meter to measure the contact angle between the droplet and the tape surface, and measure the water drop contact angle through image analysis software.

[0071] 3) Silicon-based wafer wetting time test: Select a 5cm×5cm area on the surface of a complete and flawless silicon-based wafer, remove the release film from the prepared tape and start contacting the selected area from the edge and start timing. The time it takes for the tape to completely contact and cover the wafer surface without pressure and external interference is recorded as the silicon-based wafer wetting time.

[0072] 4) Wafer cutting water seepage test: Attach the prepared tape to the wafer surface and perform the cutting operation. Then remove the tape and observe under an optical microscope whether there are water marks or residual water stains on the wafer surface caused by water seepage.

[0073] Although the present invention is disclosed as above, the protection scope of the present invention is not limited thereto. Those skilled in the art may make various changes and modifications without departing from the spirit and scope of the present invention, and these changes and modifications will fall within the protection scope of the present invention.

Claims

1. A method for preparing a silicone hybrid acrylate pressure-sensitive adhesive, characterized in that: include: Step S1: Under an inert gas protection atmosphere, copolymerizing the first mixture to obtain a silicone hybrid acrylate main glue solution; wherein, the first mixture comprises, by weight: 20-90 parts of soft monomers, 0.5-40 parts of hard monomers, 0.5-20 parts of functional monomers, 0.5-20 parts of (meth)acrylate silicone monomers, 0.5-1 parts of thermal initiators and 50-200 parts of organic solvents; Step S2: adding a second mixture to the organosilicon-hybridized acrylate main adhesive solution, mixing them evenly, and obtaining an organosilicon-hybridized acrylate pressure-sensitive adhesive; wherein, in parts by weight, the second mixture comprises: 1-50 parts of a tackifier and 1-10 parts of an antioxidant.

2. The method for preparing the organosilicon hybrid acrylate pressure-sensitive adhesive according to claim 1, characterized in that: In the step S1, the (meth)acrylate silicone monomer includes at least one of 3-(trimethoxysilyl)propyl acrylate, 3-(methoxydimethylsilyl)propyl acrylate, 3-[diethoxy(methyl)silyl]propyl methacrylate, 3-(methacryloyloxy)propyltrimethoxysilane, 3-methacryloyloxypropylmethyldimethoxysilane and 3-(methacryloyloxy)propyltriethoxysilane.

3. The method for preparing the organosilicon hybrid acrylate pressure-sensitive adhesive according to claim 1, characterized in that: In step S1, the first mixture further comprises 0.1-10 parts of an internal crosslinking agent, wherein the internal crosslinking agent comprises one of 1,3-bis(3-methacryloxypropyl)tetrakis(trimethylsiloxy)disiloxane and a polysiloxane compound having a plurality of (meth)acrylic functional end groups with double bonds.

4. The method for preparing the organosilicon hybrid acrylate pressure-sensitive adhesive according to claim 1, characterized in that: In the step S2, the second mixture further comprises 0.1-10 parts of an external crosslinking agent, and the external crosslinking agent comprises one of epoxy-terminated polysiloxane compounds, multifunctional isocyanates, multifunctional aziridines, high-valent metal acid esters and metal chelates.

5. The method for preparing the organosilicon hybrid acrylate pressure-sensitive adhesive according to claim 1, characterized in that: In the step S1, the soft monomer includes at least one of (meth) alkyl acrylates with a branched or linear structure between C7 and C15; the hard monomer includes at least one of methyl methacrylate, ethyl acrylate and isobornyl acrylate; the functional monomer includes at least one of acrylic acid, acrylamide and 2-aminoethyl methacrylate hydrochloride; the thermal initiator includes at least one of azobisisobutyronitrile, azobisisovaleronitrile, azobisisoheptylonitrile and dibenzoyl peroxide; the organic solvent includes at least one of ethyl acetate, butyl acetate, acetone, methyl ethyl ketone, benzene and toluene.

6. The method for preparing the organosilicon hybrid acrylate pressure-sensitive adhesive according to claim 1, characterized in that: In the step S2, the antioxidant includes at least one of a phenolic antioxidant, an amine antioxidant and a phosphite antioxidant, and the tackifier includes at least one of a rosin resin, a hydrocarbon and a terpene resin.

7. The method for preparing the organosilicon hybrid acrylate pressure-sensitive adhesive according to claim 1, characterized in that: In the step S1, the copolymerization reaction is carried out at a temperature of 60-90°C and for a time of 8-14 hours.

8. A method for preparing a pressure-sensitive adhesive tape, characterized in that: include: Step M1: coating the organosilicon hybrid acrylate pressure-sensitive adhesive on the base film (1), and drying the base film to obtain a pressure-sensitive adhesive layer (2); the organosilicon hybrid acrylate pressure-sensitive adhesive is prepared by the preparation method of the organosilicon hybrid acrylate pressure-sensitive adhesive according to any one of claims 1 to 7; Step M2: affixing a release film (3) to the surface of the pressure-sensitive adhesive layer (2) to obtain a pressure-sensitive adhesive tape.

9. The method for preparing the UV adhesive tape according to claim 8, characterized in that: In the step M1, the thickness of the base film (1) is 50-200 μm, and the thickness of the pressure-sensitive adhesive layer (2) is 5-50 μm.

10. The method for preparing the UV anti-viscosity tape according to claim 8, characterized in that: In the step M1, the material of the base film (1) is selected from one of polypropylene, polyethylene, polyolefin, polyethylene terephthalate and polyvinyl chloride.

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