Epoxy modified acrylic resin for photoetching slurry

Abstract

The epoxy modified acrylic resin is prepared by the following steps: pouring 30 parts of ethylene glycol butyl ether into a reaction kettle, introducing inert gas, and heating to 80-90 DEG C in an oil bath; uniformly mixing 8-12 parts of monomer methacrylic acid, 8-12 parts of monomer n-butyl acrylate, 8-12 parts of monomer hydroxyethyl methylacrylate, 0.4-06 parts of peroxide initiator, 0.1-0.2 part of aliphatic mercaptan and 8-12 parts of ethylene glycol butyl ether, dropwise adding the mixture into the reaction kettle, and preserving heat; uniformly mixing 0.4-0.6 part of peroxide initiator and 2-4 parts of ethylene glycol butyl ether, and dropwise adding the mixture into the reaction kettle within 1-3 hours after the mixture is completely dissolved; introducing oxygen into the reaction kettle, keeping the temperature at 85-95 DEG C, and adding 0.1-0.3 part of hydroquinone until the hydroquinone is completely dissolved; the curing agent is high in crosslinking degree after being cured, has good thermal stability, weather resistance and heat resistance, and has good resolution in photoetching electronic products.

Description

Technical Field

[0001] The invention relates to the technical field of acrylic resins, and in particular to an epoxy-modified acrylic resin for photolithography slurry. Background Art

[0002] As the integration of electronic components becomes higher and higher, and they are made smaller and smaller, the various circuits on the components are also required to be thinner and thinner, and traditional methods can no longer meet the requirements. As a more efficient and environmentally friendly method, ultraviolet lithography technology is increasingly used in micro-nano devices, but the corresponding resins are basically sourced from Japan and South Korea, with very few selectivities. This invention is a new type of epoxy acrylic (alkali-soluble) resin, which has a photosensitive group and an alkali-soluble group, a high degree of cross-linking after curing, and good thermal stability and weather resistance. Summary of the invention

[0003] The present invention aims to provide an epoxy-modified acrylic resin for photolithography slurry, which has a high degree of crosslinking after curing, good thermal stability and weather resistance, good heat resistance, and good resolution in photolithography electronic products.

[0004] To achieve the above object, the technical solution adopted by the present invention is: an epoxy-modified acrylic resin for photolithography slurry is obtained by the following steps: Step 1: Pour 30 parts of ethylene glycol butyl ether into a reaction kettle, introduce inert gas, and heat in an oil bath to 80-90°C; Step 2: Evenly mix 10 parts of methacrylic acid, 10 parts of n-butyl acrylate, 10 parts of hydroxyethyl methacrylate, 0.5 parts of peroxide initiator, 0.15 parts of aliphatic mercaptan, and 10 parts of ethylene glycol butyl ether, and dropwise add the mixture into a reaction kettle for heat preservation; Step 3: Evenly mix 0.5 parts of peroxide initiator and 3 parts of ethylene glycol butyl ether, and add dropwise to the reactor within 1 to 3 hours after the mixture is completely dissolved; Step 4: After the addition is completed, keep the temperature for 2 hours. After the temperature rises to 90-100°C, take the solution to test infrared. There is no peak at 1635 (cm⁻¹)-1638 (cm⁻¹) and no characteristic peak of carbon-carbon double bond. The first step is completed. Step 5: introduce oxygen into the reactor, maintain the temperature at 85-95°C, add 0.2 parts of hydroquinone and dissolve it completely; Step 6: Mix 0.5 parts of triphenylphosphine and 3.15 parts of ethylene glycol butyl ether evenly, add dropwise to the reaction kettle within 1 hour after the mixture is completely dissolved, and keep warm for 0.5 to 1.5 hours; Step 7: Evenly mix 15 parts of 2,3-epoxypropyl methacrylate and 17 parts of ethylene glycol butyl ether, add dropwise within 5 hours, and keep warm for 2-4 hours; then raise the temperature to 95-105°C, keep warm for 4-6 hours, take the solution for infrared testing, there is no characteristic peak of epoxy group near 910 (cm⁻¹), and the polymerization is complete.

[0005] The technical solution further improved in the above technical solution is as follows: 1. In the above scheme, the inert gas is nitrogen.

[0006] 2. In the above scheme, the stirring speed of step 1 is 150~250r / min.

[0007] 3. In the above scheme, the temperature is raised to 90-100°C and the holding time is 3-5h in step 4.

[0008] 4. In the above scheme, the insulation time of step 2 is 1 to 3 hours.

[0009] 5. In the above scheme, the dropping time of step 2 is 4 to 6 hours.

[0010] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art: The epoxy modified acrylic resin used for photolithography slurry of the present invention has a high degree of crosslinking after curing, good thermal stability and weather resistance, good heat resistance, and good resolution in photolithography electronic products. BRIEF DESCRIPTION OF THE DRAWINGS

[0011] Attached Figure 1 The infrared spectrum of the synthesis process of the epoxy-modified acrylic resin used for photolithography slurry of the present invention; Attached Figure 2 The GPC spectrum of the epoxy-modified acrylic resin used in the photolithography slurry of the present invention. DETAILED DESCRIPTION

[0011] The present invention can be further understood through the specific embodiments given below, but they are not intended to limit the present invention.

[0012] Embodiment: An epoxy-modified acrylic resin for photolithography slurry is obtained by the following steps: Step 1: Pour 30 parts of ethylene glycol butyl ether into a reaction kettle, introduce inert gas, and heat in an oil bath to 80-90°C; Step 2: Evenly mix 10 parts of methacrylic acid, 10 parts of n-butyl acrylate, 10 parts of hydroxyethyl methacrylate, 0.5 parts of peroxide initiator, 0.15 parts of aliphatic mercaptan, and 10 parts of ethylene glycol butyl ether, and dropwise add the mixture into a reaction kettle for heat preservation; Step 3: Evenly mix 0.5 parts of peroxide initiator and 3 parts of ethylene glycol butyl ether, and add dropwise to the reactor within 1 to 3 hours after the mixture is completely dissolved; Step 4: After the addition is completed, keep the temperature for 2 hours. After the temperature rises to 95°C, take the solution to test the infrared. There is no peak at 1635 (cm⁻¹)-1638 (cm⁻¹) and no characteristic peak of carbon-carbon double bond. The first step is completed. Step 5: introduce oxygen into the reactor, maintain the temperature at 90°C, add 0.2 parts of hydroquinone and dissolve it completely; Step 6: Mix 0.5 parts of triphenylphosphine and 3.15 parts of ethylene glycol butyl ether evenly, add dropwise to the reaction kettle within 1 hour after the mixture is completely dissolved, and keep warm for 1 hour; Step 7: Evenly mix 15 parts of 2,3-epoxypropyl methacrylate and 17 parts of ethylene glycol butyl ether, add dropwise within 5 hours, and keep warm for 3 hours; then raise the temperature to 100°C and keep warm for 5 hours. Take the solution for infrared testing. There is no characteristic peak of epoxy group near 910 (cm⁻¹), and the polymerization is complete.

[0013] The above-mentioned inert gas is nitrogen.

[0014] The stirring speed in the above step 1 is 200 r / min.

[0015] In the above step 4, the temperature is raised to 95°C and the holding time is 4 hours.

[0016] The insulation time of the above step 2 is 2h.

[0017] The dropping time of the above step 2 is 5h.

[0018] Infrared spectrum of the synthesis process, such as Figure 1 Said: There is no peak at 1635 (cm⁻¹)-1638 (cm⁻¹) and no characteristic peak of carbon-carbon double bond, and the first step is completed.

[0019] There is no characteristic peak of epoxy group near 910 (cm⁻¹), and the second step is completed.

[0020] GPC spectrum, such as Figure 2 As shown: The weight average molecular weight MW is 15854, the polydispersity coefficient PD is 3.08, and the degree of polymerization is relatively high.

[0021] Test acid value Acid value definition: Acid value is defined as the number of milligrams of potassium hydroxide required to neutralize 1g of resin, so the acid value is expressed in "mgKOH / g". Generally speaking, the smaller the acid value, the higher the degree of resin reaction. The acid value is the mass of potassium hydroxide required to titrate 1 gram of the sample to be tested. The formula is: IA=A*N*56.1 / W IA is in milligrams, A is the titration of potassium hydroxide in ml, N is the equivalent concentration of potassium hydroxide, 56.1 is the molecular weight of potassium hydroxide, and W is the mass of the analyte in grams.

[0022] Test acid value: 50mgKOH / g.

[0023] When the epoxy-modified acrylic resin used in the photolithography slurry is used, the degree of cross-linking after curing is high, and the resin has good thermal stability, weather resistance, and heat resistance, and has good resolution in photolithography electronic products.

[0024] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. An epoxy-modified acrylic resin for photolithography slurry, characterized in that: Obtained by the following steps: Step 1: Pour 30 parts of ethylene glycol butyl ether into a reaction kettle, introduce inert gas, and heat in an oil bath to 80-90°C; Step 2: Evenly mix 8-12 parts of methacrylic acid monomer, 8-12 parts of n-butyl acrylate monomer, 8-12 parts of hydroxyethyl methacrylate monomer, 0.4-06 parts of peroxide initiator, 0.1-0.2 parts of aliphatic mercaptan, and 8-12 parts of ethylene glycol butyl ether, and dropwise add to the reaction kettle for heat preservation; Step 3: Evenly mix 0.4-0.6 parts of peroxide initiator and 2-4 parts of ethylene glycol butyl ether, and add dropwise to the reactor within 1-3 hours after the mixture is completely dissolved; Step 4: After the addition is completed, keep the temperature for 1-3 hours, raise the temperature to 90-100℃ and keep the temperature, take the solution to test infrared, there is no peak at 1635 (cm⁻¹)-1638 (cm⁻¹) and no characteristic peak of carbon-carbon double bond, the first step is completed; Step 5: introduce oxygen into the reactor, maintain the temperature at 85-95°C, add 0.1-0.3 parts of hydroquinone and dissolve it completely; Step 6: Evenly mix 0.4-0.6 parts of triphenylphosphine and 3-3.3 parts of ethylene glycol butyl ether, and add dropwise to the reaction kettle within 0.5-1.5 hours after the mixture is completely dissolved, and keep warm for 0.5-1.5 hours; Step 7: Evenly mix 14-16 parts of 2,3-epoxypropyl methacrylate and 16-18 parts of ethylene glycol butyl ether, add dropwise within 4-6 hours, and keep warm for 2-4 hours; then raise the temperature to 95-105°C, keep warm for 4-6 hours, take the solution for infrared testing, there is no characteristic peak of epoxy group near 910 (cm⁻¹), and the polymerization is complete.

2. The epoxy-modified acrylic resin for photolithography slurry according to claim 1, characterized in that: The inert gas is nitrogen.

3. The epoxy-modified acrylic resin for photolithography slurry according to claim 1, characterized in that: The stirring speed of step 1 is 150-250 r / min.

4. The epoxy-modified acrylic resin for photolithography slurry according to claim 1, characterized in that: In the step 4, the temperature is raised to 90-100° C. and the holding time is 3-5 hours.

5. The epoxy-modified acrylic resin for photolithography slurry according to claim 1, characterized in that: The insulation time of step 2 is 1 to 3 hours.

6. The epoxy-modified acrylic resin for photolithography slurry according to claim 1, characterized in that: The dropping time of step 2 is 4 to 6 hours.

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