Production process of silicon wafer cutting fluid

Abstract

The present invention provides a production process for a silicon wafer cutting fluid, relating to the technical field of cutting fluids. The production process for the cutting fluid comprises the following steps: 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 are mixed to form the silicon wafer cutting fluid; preparation of the wetting agent comprises the following steps: S11: reacting phytic acid and allyl glycidyl ether to obtain a prepolymer; and S12: polymerizing the prepolymer with N,N-dimethylacrylamide, glutaconic acid, and an initiator to obtain the dispersant. The cutting fluid produced effectively improves the qualified rate of cutting large-size silicon wafers.

Description

Technical Field

[0001] The present invention relates to the technical field of cutting fluids, and in particular to a production process of silicon wafer cutting fluids. 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 for 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 for silicon wafer cutting fluid, the production process for silicon wafer cutting fluid comprising the following steps:

[0005] The silicon wafer cutting fluid is formed by mixing 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;

[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 utilizes modified phytic acid to obtain a wetting agent, which, under weakly alkaline conditions, can exert electrostatic repulsion on the surface of negatively charged silicon powder particles. Based on this, the hydroxyl groups of the phytic acid react with the epoxy groups of allyl glycidyl ether, and then undergo free radical polymerization with N,N-dimethylacrylamide and glutaconic acid to obtain a long carbon chain. The tertiary amine groups in the N,N-dimethylacrylamide and the carboxyl groups on the glutaconic acid can be relatively stably anchored to the silicon powder, allowing the wetting agent to effectively spread around the silicon powder, achieving a good wetting effect. Furthermore, the phytic acid can chelate and remove existing metal ions, preventing metal ion contamination and improving the quality of the cut silicon wafers.

[0021] The dispersant is modified with chitosan oligosaccharide with a positive charge in the solution. The amino group on the surface of chitosan oligosaccharide has a good anchoring effect. By grafting a certain amount of pentaerythritol tetraacrylate, a network-like molecular structure can be obtained, which effectively reduces the surface tension of water and has good defoaming ability. The ester bond 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 agglomeration. Finally, grafting with dodecyl glycidyl ether can significantly reduce the surface tension of the chitosan oligosaccharide solution, making the chitosan oligosaccharide amphiphilic and playing a good dispersing role. 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. Those skilled in the art will readily understand the other advantages and benefits of the present invention from the disclosure herein. The present invention may also be implemented or applied through various other specific embodiments, and the details in this specification may be modified or altered 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., glutaconic 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 for 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 and reacting 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, 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, wherein 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, and the reaction is carried out under nitrogen protection. The obtained product is washed with water and ethanol and then 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, wherein 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, the reaction is cooled, filtered, washed, and vacuum-dried to obtain a first reactant;

[0032] S22: reacting the first reactant and pentaerythritol tetraacrylate in K2S2O8 (0.2% by weight of the total reactant) under nitrogen protection to obtain a second reactant, wherein the weight ratio of the first reactant to the pentaerythritol tetraacrylate is 1:1, the reaction temperature is 60° C., and the reaction time is 24 hours. After the reaction, the second reactant is cooled, filtered, washed, and vacuum-dried 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 reactants. 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 for 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 and reacting 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, 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, wherein 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, and the reaction is carried out under nitrogen protection. The obtained product is washed with water and ethanol and then 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, wherein 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, the reaction is cooled, filtered, washed, and vacuum-dried to obtain a first reactant;

[0042] S22: reacting the first reactant and pentaerythritol tetraacrylate in K2S2O8 (0.2% by weight of the total reactant) 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., and the reaction time is 24 hours. After the reaction, the second reactant is cooled, filtered, washed, and vacuum-dried 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 for 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 and reacting 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, 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, wherein 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, and the reaction is carried out under nitrogen protection. The obtained product is washed with water and ethanol and then 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, wherein 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, the reaction is cooled, filtered, washed, and vacuum-dried to obtain a first reactant;

[0052] S22: reacting the first reactant and pentaerythritol tetraacrylate in K2S2O8 (0.2% by weight of the total reactant) under nitrogen protection to obtain a second reactant, wherein the weight ratio of the first reactant to the pentaerythritol tetraacrylate is 1:1, the reaction temperature is 60° C., and the reaction time is 24 hours. After the reaction, the second reactant is cooled, filtered, washed, and vacuum-dried 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 reactants. 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 for 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 and reacting 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, wherein 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, and the reaction is carried out under nitrogen protection. The obtained product is washed with water and ethanol and then 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, wherein 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, the reaction is cooled, filtered, washed, and vacuum-dried to obtain a first reactant;

[0062] The first reactant and dodecyl glycidyl ether are reacted in an alkaline aqueous solution, wherein 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 a 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 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. 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 shown in Table 1, the cutting fluids of Examples 1 to 3 of the present invention all 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 bridging of adsorption sites between chitosan oligosaccharides.

[0070] Therefore, the present invention effectively overcomes the various shortcomings of the prior art and has high industrial value. The above embodiments are merely illustrative of the principles and effects of the present invention and are not intended to limit the present invention. Anyone skilled in the art may modify or alter the above embodiments without departing from the spirit and scope of the present invention. Therefore, all equivalent modifications or alterations made by persons of ordinary skill in the art without departing from the spirit and technical concepts disclosed herein are intended to 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: The silicon wafer cutting fluid is prepared by mixing 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, by weight; 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 to N,N-dimethylacrylamide and glutaric 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 process for producing a silicon wafer cutting fluid according to claim 1, wherein: The weight ratio of the second reactant to the dodecyl glycidyl ether is (5-10):

1.

8. The process for producing a silicon wafer cutting fluid according to claim 1, wherein: The stabilizer is any one of diethanolamine and triethanolamine.

9. The silicon wafer cutting fluid prepared according to the production process of silicon wafer cutting fluid according to any one of claims 1 to 8.

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