Production process of silicon wafer cutting fluid
By modifying materials such as phytic acid and allyl glycidyl ether, wet and dispersant are prepared, which solves the problem of insufficient wetting and dispersion performance of large-sized silicon wafer cutting fluid, and achieves efficient silicon wafer cutting effect, overcomes the Cutting quality problems in the prior art.
Patent Information
- Application Number
- CN202411237672.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-05
- Publication Date
- 2024-12-10
- Estimated Expiration
- 2044-09-05
AI Technical Summary
During the cutting process, large-sized silicon wafers are not wet and dispersed, resulting in cutting quality problems, and existing cutting liquids are difficult to meet.
Wetting agents and dispersants are prepared by modified phytic acid and allyl glycidyl ether. The wetting and dispersing effect is improved through electrostatic repulsion and network-like molecular structure, and the pH is adjusted with a stabilizer to form an efficient silicon wafer cutting solution. .
It significantly improves the wetting effect and dispersion performance of the silicon wafer cutting liquid, improves the cutting quality and performance, reduces metal ion pollution, and improves the overall performance of the cutting liquid.
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Figure BDA0005028220830000051
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of cutting fluid, and in particular to a production process of silicon wafer cutting fluid. Background Art
[0002] The large-size 210 silicon wafer has an area 60% larger than that of the conventional 166 silicon wafer. Conventional cutting methods and cutting liquids are difficult to meet the normal cutting requirements of large-size silicon wafers. The center of the silicon wafer is prone to quality problems due to insufficient wetting and dispersion properties of the cutting liquid. Summary of the invention
[0003] The purpose of the present invention is to overcome the defects of the prior art and provide a production process of silicon wafer cutting fluid, which can solve the problems existing in the prior art when cutting large-size silicon wafers.
[0004] In order to achieve the above and other purposes, the present invention is implemented by including the following technical solutions: The present invention provides a production process of silicon wafer cutting fluid, and the silicon wafer cutting fluid production process includes the following steps:
[0005] Mix 10 to 15 parts of a wetting agent, 20 to 30 parts of a dispersant, 6 to 10 parts of a stabilizer and 40 to 60 parts of pure water to form the silicon wafer cutting fluid;
[0006] The preparation of the wetting agent comprises the following steps:
[0007] S11: reacting phytic acid and allyl glycidyl ether to obtain a prepolymer;
[0008] S12: polymerizing the prepolymer, N,N-dimethylacrylamide, glutaconic acid and an initiator to obtain the wetting agent;
[0009] The preparation of the dispersant comprises the following steps:
[0010] S21: reacting chitosan oligosaccharide with maleic anhydride to obtain a first reactant;
[0011] S22: reacting the first reactant with pentaerythritol tetraacrylate and an initiator to obtain a second reactant;
[0012] S23: reacting the second reactant with dodecyl glycidyl ether to obtain the dispersant.
[0013] In some embodiments, the initiator includes any one of potassium persulfate, benzoyl peroxide, or an azo compound.
[0014] In some embodiments, in S11, the molar ratio of the phytic acid to the allyl glycidyl ether is 1:(4-6).
[0015] In some embodiments, in S12, the weight ratio of the prepolymer, N,N-dimethylacrylamide and glutaconic acid is (2-3):1:(0.8-1.2).
[0016] In some embodiments, in S21, the weight ratio of the chitosan oligosaccharide to the maleic anhydride is 1:(0.5-1).
[0017] In some embodiments, the weight ratio of the first reactant to the pentaerythritol tetraacrylate is (1-2):1.
[0018] In some embodiments, the weight ratio of the second reactant to the dodecyl glycidyl ether is (5-10):1.
[0019] In some embodiments, the stabilizer is any one of diethanolamine and triethanolamine.
[0020] The present invention adopts the method of modifying phytic acid to obtain a wetting agent, which can have an electrostatic repulsion effect with silicon powder particles with negative charges on the surface under weak alkaline conditions, and on this basis, the hydroxyl group of phytic acid and the epoxy group of allyl glycidyl ether are reacted, and then free radical polymerization is performed with N, N-dimethylacrylamide and glutaconic acid to obtain a long carbon chain, wherein the tertiary amine group in N, N-dimethylacrylamide and the carboxyl group on glutaconic acid can be relatively stably anchored on the silicon powder, that is, the wetting agent can be effectively spread around the silicon powder, and a good wetting effect is achieved. In addition, phytic acid can chelate and remove existing metal ions, prevent metal ion pollution, and also improve the quality of cut silicon wafers.
[0021] The dispersant is modified with chitosan oligosaccharide with positive charge in the solution. The amino group on the surface of chitosan oligosaccharide has a good anchoring effect. A network-like molecular structure can be obtained by grafting a certain amount of pentaerythritol tetraacrylate, which effectively reduces the surface tension of water and has good defoaming ability. The ester bonds on pentaerythritol tetraacrylate can effectively occupy part of the adsorption sites on the surface of chitosan oligosaccharide, reduce the bridging between chitosan oligosaccharide molecules, and effectively prevent chitosan oligosaccharide from agglomerating. Finally, grafting with dodecyl glycidyl ether can significantly reduce the surface tension of the chitosan oligosaccharide solution, making the chitosan oligosaccharide amphiphilic and having a good dispersing effect. The stabilizer can adjust the pH of the cutting fluid to improve the performance of the cutting fluid to a certain extent. DETAILED DESCRIPTION
[0022] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.
[0023] In the following examples, phytic acid was purchased from Sigma-Aldrich (Shanghai) Trading Co., Ltd., allyl glycidyl ether was purchased from Shanghai MacLean Biochemical Technology Co., Ltd., N,N-dimethylacrylamide was purchased from Qingdao Reinars Polymer Materials Co., Ltd., glutaric acid was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd., chitosan oligosaccharide was purchased from Shanghai MacLean Biochemical Technology Co., Ltd. (CAS: 148411-57-8), maleic anhydride was purchased from Shanghai MacLean Biochemical Technology Co., Ltd., pentaerythritol tetraacrylate was purchased from Wuhan Rongcan Biotechnology Co., Ltd. (CAS: 4986-89-4), and dodecyl glycidyl ether was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd. (CAS: 2461-18-9).
[0024] Example 1
[0025] A production process of a silicon wafer cutting fluid, the silicon wafer cutting fluid comprising the following components in parts by weight:
[0026] 10 parts of wetting agent, 20 parts of dispersant, 6 parts of stabilizer (diethanolamine), and 40 parts of pure water.
[0027] Wherein, the preparation of the wetting agent comprises the following steps:
[0028] S11: stirring phytic acid and allyl glycidyl ether at 25° C. for 1 hour to obtain a prepolymer, wherein the molar ratio of phytic acid to allyl glycidyl ether is 1:4;
[0029] S12: The prepolymer and N,N-dimethylacrylamide, glutaconic acid and 0.3% of the total mass of K2S2O8 of the reactants are polymerized in water to obtain the wetting agent, the weight ratio of the prepolymer, N,N-dimethylacrylamide and glutaconic acid is 2:1:0.8, the weight of water is 3 times the total weight of the reactants, the reaction temperature is 70°C, the reaction is carried out under nitrogen protection, and the product is washed with water and ethanol and freeze-dried for 24 hours to obtain the final wetting agent.
[0030] The preparation of the dispersant comprises the following steps:
[0031] S21: chitosan oligosaccharide, maleic anhydride and N, N-dimethylformamide are reacted to obtain a first reactant, the weight ratio of chitosan oligosaccharide to maleic anhydride is 1:0.5, the weight of N, N-dimethylformamide is 3 times that of the reactant, the reaction temperature is 60° C., the reaction time is 10 hours, and after the reaction is completed, cooling, filtering, washing, and vacuum drying are performed to obtain a first reactant;
[0032] S22: reacting the first reactant and pentaerythritol tetraacrylate in K2S2O8 with a total weight of 0.2% under nitrogen protection to obtain a second reactant, wherein the weight ratio of the first reactant to pentaerythritol tetraacrylate is 1:1, the reaction temperature is 60° C., the reaction time is 24 hours, and after the reaction is completed, cooling, filtering, washing, and vacuum drying are performed to obtain the second reactant;
[0033] S23: reacting the second reactant and dodecyl glycidyl ether in an alkaline aqueous solution, wherein the weight ratio of the second reactant to dodecyl glycidyl ether is 5:1, the reaction temperature is 80°C, the reaction time is 24 hours, the alkaline aqueous solution is 20% sodium hydroxide solution, and the weight of the alkaline aqueous solution is 4 times that of the reactant. After the reaction is completed, the product is cooled, filtered, washed, and vacuum dried to obtain the dispersant.
[0034] Example 2
[0035] A production process of a silicon wafer cutting fluid, the silicon wafer cutting fluid comprising the following components in parts by weight:
[0036] 15 parts of wetting agent, 30 parts of dispersant, 10 parts of stabilizer (diethanolamine), and 60 parts of pure water.
[0037] Wherein, the preparation of the wetting agent comprises the following steps:
[0038] S11: stirring phytic acid and allyl glycidyl ether at 25° C. for 1 hour to obtain a prepolymer, wherein the molar ratio of phytic acid to allyl glycidyl ether is 1:6;
[0039] S12: The prepolymer and N,N-dimethylacrylamide, glutaconic acid and 0.3% of the total mass of K2S2O8 of the reactants are polymerized in water to obtain the wetting agent, the weight ratio of the prepolymer, N,N-dimethylacrylamide and glutaconic acid is 3:1:1.2, the weight of water is 3 times the total weight of the reactants, the reaction temperature is 70°C, the reaction is carried out under nitrogen protection, and the product is washed with water and ethanol and freeze-dried for 24 hours to obtain the final wetting agent.
[0040] The preparation of the dispersant comprises the following steps:
[0041] S21: chitosan oligosaccharide, maleic anhydride and N, N-dimethylformamide are reacted to obtain a first reactant, the weight ratio of chitosan oligosaccharide to maleic anhydride is 1:1, the weight of N, N-dimethylformamide is 3 times that of the reactant, the reaction temperature is 60° C., the reaction time is 10 hours, and after the reaction is completed, cooling, filtering, washing, and vacuum drying are performed to obtain the first reactant;
[0042] S22: reacting the first reactant and pentaerythritol tetraacrylate in K2S2O8 with a total weight of 0.2% under nitrogen protection to obtain a second reactant, wherein the weight ratio of the first reactant to pentaerythritol tetraacrylate is 2:1, the reaction temperature is 60° C., the reaction time is 24 hours, and after the reaction is completed, cooling, filtering, washing, and vacuum drying are performed to obtain the second reactant;
[0043] S23: reacting the second reactant and dodecyl glycidyl ether in an alkaline aqueous solution, wherein the weight ratio of the second reactant to dodecyl glycidyl ether is 10:1, the reaction temperature is 80°C, the reaction time is 24 hours, the alkaline aqueous solution is 20% sodium hydroxide solution, and the weight of the alkaline aqueous solution is 4 times that of the reactants. After the reaction is completed, the product is cooled, filtered, washed, and vacuum dried to obtain the dispersant.
[0044] Example 3
[0045] A production process of a silicon wafer cutting fluid, the silicon wafer cutting fluid comprising the following components in parts by weight:
[0046] 12 parts of wetting agent, 25 parts of dispersant, 8 parts of stabilizer (diethanolamine), and 50 parts of pure water.
[0047] Wherein, the preparation of the wetting agent comprises the following steps:
[0048] S11: stirring phytic acid and allyl glycidyl ether at 25° C. for 1 hour to obtain a prepolymer, wherein the molar ratio of phytic acid to allyl glycidyl ether is 1:4;
[0049] S12: The prepolymer and N,N-dimethylacrylamide, glutaconic acid and 0.3% of the total mass of K2S2O8 of the reactants are polymerized in water to obtain the wetting agent, the weight ratio of the prepolymer, N,N-dimethylacrylamide and glutaconic acid is 2:1:0.8, the weight of water is 3 times the total weight of the reactants, the reaction temperature is 70°C, the reaction is carried out under nitrogen protection, and the product is washed with water and ethanol and freeze-dried for 24 hours to obtain the final wetting agent.
[0050] The preparation of the dispersant comprises the following steps:
[0051] S21: chitosan oligosaccharide, maleic anhydride and N, N-dimethylformamide are reacted to obtain a first reactant, the weight ratio of chitosan oligosaccharide to maleic anhydride is 1:0.5, the weight of N, N-dimethylformamide is 3 times that of the reactant, the reaction temperature is 60° C., the reaction time is 10 hours, and after the reaction is completed, cooling, filtering, washing, and vacuum drying are performed to obtain a first reactant;
[0052] S22: reacting the first reactant and pentaerythritol tetraacrylate in K2S2O8 with a total weight of 0.2% under nitrogen protection to obtain a second reactant, wherein the weight ratio of the first reactant to pentaerythritol tetraacrylate is 1:1, the reaction temperature is 60° C., the reaction time is 24 hours, and after the reaction is completed, cooling, filtering, washing, and vacuum drying are performed to obtain the second reactant;
[0053] S23: reacting the second reactant and dodecyl glycidyl ether in an alkaline aqueous solution, wherein the weight ratio of the second reactant to dodecyl glycidyl ether is 5:1, the reaction temperature is 80°C, the reaction time is 24 hours, the alkaline aqueous solution is 20% sodium hydroxide solution, and the weight of the alkaline aqueous solution is 4 times that of the reactant. After the reaction is completed, the product is cooled, filtered, washed, and vacuum dried to obtain the dispersant.
[0054] Comparative Example 1
[0055] A production process of a silicon wafer cutting fluid, the silicon wafer cutting fluid comprising the following components in parts by weight:
[0056] 10 parts of wetting agent, 20 parts of dispersant, 6 parts of stabilizer (diethanolamine), and 40 parts of pure water.
[0057] Wherein, the preparation of the wetting agent comprises the following steps:
[0058] S11: stirring phytic acid and allyl glycidyl ether at 25° C. for 1 hour to obtain a prepolymer, wherein the molar ratio of phytic acid to allyl glycidyl ether is 1:4;
[0059] S12: The prepolymer and N,N-dimethylacrylamide, glutaconic acid and 0.3% of the total mass of K2S2O8 of the reactants are polymerized in water to obtain the wetting agent, the weight ratio of the prepolymer, N,N-dimethylacrylamide and glutaconic acid is 2:1:0.8, the weight of water is 3 times the total mass of the reactants, the reaction temperature is 70°C, the reaction is carried out under nitrogen protection, and the product is washed with water and ethanol and freeze-dried for 24 hours to obtain the final wetting agent.
[0060] The preparation of the dispersant comprises the following steps:
[0061] S21: chitosan oligosaccharide, maleic anhydride and N, N-dimethylformamide are reacted to obtain a first reactant, the weight ratio of chitosan oligosaccharide to maleic anhydride is 1:0.5, the weight of N, N-dimethylformamide is 3 times that of the reactant, the reaction temperature is 60° C., the reaction time is 10 hours, and after the reaction is completed, cooling, filtering, washing, and vacuum drying are performed to obtain a first reactant;
[0062] The first reactant and dodecyl glycidyl ether are reacted in an alkaline aqueous solution, the weight ratio of the first reactant to dodecyl glycidyl ether is 5:1, the reaction temperature is 80° C., the reaction time is 24 hours, the alkaline aqueous solution is 20% sodium hydroxide solution, and the weight of the alkaline solution is 4 times that of the reactant. After the reaction is completed, the product is cooled, filtered, washed, and vacuum dried to obtain the dispersant.
[0063] Comparative Example 2
[0064] Comparative Example 2 is a commercially available Yitian cutting fluid.
[0065] The cutting fluids obtained in Examples 1 to 3 and Comparative Examples 1 to 2 were used for cutting on the same cutting machine under the same cutting process conditions, and the number of cut pieces, qualified rate, wire breakage rate, and contamination rate were measured or counted. The results are shown in Table 1.
[0066] Table 1 Cutting performance comparison table
[0067]
[0068]
[0069] As can be seen from Table 1, the cutting fluids of Examples 1 to 3 of the present invention have better cutting performance data than the cutting fluids of Comparative Examples 1 to 2 under the same cutting process conditions. Since Examples 1 to 3 of the present invention have good wetting effects and strong dispersion effects, the corresponding silicon wafer cutting effects are good. The poor effect of Comparative Example 1 may be due to sedimentation and other problems caused by the bridging of adsorption sites between chitosan oligosaccharides.
[0070] Therefore, the present invention effectively overcomes various shortcomings in the prior art and has a high industrial utilization value. The above embodiments are only illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the technology can modify or change the above embodiments without violating the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical ideas disclosed by the present invention should still be covered by the claims of the present invention.
Claims
1. A production process for silicon wafer cutting fluid, characterized in that: The production process comprises the following steps: Mix 10 to 15 parts of a wetting agent, 20 to 30 parts of a dispersant, 6 to 10 parts of a stabilizer and 40 to 60 parts of pure water to form the silicon wafer cutting fluid; The preparation of the wetting agent comprises the following steps: S11: reacting phytic acid and allyl glycidyl ether to obtain a prepolymer; S12: polymerizing the prepolymer, N,N-dimethylacrylamide, glutaconic acid and an initiator to obtain the wetting agent; The preparation of the dispersant comprises the following steps: S21: reacting chitosan oligosaccharide with maleic anhydride to obtain a first reactant; S22: reacting the first reactant with pentaerythritol tetraacrylate and an initiator to obtain a second reactant; S23: reacting the second reactant with dodecyl glycidyl ether to obtain the dispersant.
2. The production process of silicon wafer cutting fluid according to claim 1, characterized in that: The initiator includes any one of potassium persulfate, benzoyl peroxide or an azo compound.
3. The production process of silicon wafer cutting fluid according to claim 1, characterized in that: In S11, the molar ratio of the phytic acid to the allyl glycidyl ether is 1:(4-6).
4. The production process of silicon wafer cutting fluid according to claim 1, characterized in that: In S12, the weight ratio of the prepolymer, N,N-dimethylacrylamide and glutaconic acid is (2-3):1:(0.8-1.2).
5. The production process of silicon wafer cutting fluid according to claim 1, characterized in that: In S21, the weight ratio of the chitosan oligosaccharide to the maleic anhydride is 1:(0.5-1).
6. The production process of silicon wafer cutting fluid according to claim 1, characterized in that: The weight ratio of the first reactant to the pentaerythritol tetraacrylate is (1-2):
1.
7. The production process of silicon wafer cutting fluid according to claim 1, characterized in that: The weight ratio of the second reactant to the dodecyl glycidyl ether is (5-10):
1.
8. The production process of silicon wafer cutting fluid according to claim 1, characterized in that: The stabilizer is any one of diethanolamine and triethanolamine.
9. The silicon wafer cutting fluid prepared according to any one of the production processes of silicon wafer cutting fluids according to claims 1 to 8.
Citation Information
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