Preparation process of aluminum oxide composite polishing solution for diamond substrate

Abstract

The invention relates to the technical field of polishing solutions, and discloses a preparation process of an aluminum oxide composite polishing solution for a diamond substrate, and the aluminum oxide composite polishing solution comprises the following formula raw materials: a polishing solution, diethylene glycol monobutyl ether, alkylphenol polyoxyethylene, No. 5 white mineral oil, No. 10 white mineral oil, ethylene glycol monooctyl ether, deionized water and the like. According to the aluminum oxide composite polishing solution for the diamond substrate, diethylene glycol monobutyl ether with high chemical energy is adopted, the cleaning effect of the polishing solution is improved, the production efficiency of the polishing solution is enhanced, a large number of fracture structures and elastic structures with micro cracks are formed in the polishing solution, and fracture energy generated in the deformation process can be absorbed; and the block copolymer is an amphiphilic polymer, and the hydrophilic and oleophylic amphipathicity of the polishing solution is enhanced through the synergistic effect of the block copolymer and the carboxyl group on the graphene.

Description

Technical Field

[0001] The invention relates to the technical field of polishing liquid, in particular to a preparation process of an aluminum oxide composite polishing liquid for a diamond substrate. Background Art

[0002] At present, diamond and polysilicon are used more and more widely, and the related thinning and polishing processes are becoming more and more sophisticated and the requirements are becoming more and more stringent. The base liquid of the commonly used diamond polishing grinding fluid is mainly based on polyols and water as solvents, and is emulsified with an emulsifier before use. Its advantage is that it is low-cost and easy to promote.

[0003] In addition, the quality of ordinary polishing liquid is poor, which causes the polishing liquid to easily heat up and have poor lubrication ability during actual application, which can easily cause scratches on the grinding body. The batching and stirring process of the grinding polishing liquid during the production process will directly affect the quality of the polishing liquid. However, the compatibility of flexible molecules in the material is poor, resulting in uneven dispersion and reducing the quality of the polishing liquid. Summary of the invention

[0004] 1. Technical issues to be resolved

[0005] In view of the shortcomings of the prior art, the present invention provides a process for preparing an alumina composite polishing liquid for a diamond substrate, which solves the problem that the quality of ordinary polishing liquid is poor, resulting in poor adhesion of the polishing liquid on the coating during actual application, and at the same time solves the problem that the flexible molecule modified polyurethane material has poor compatibility in the material, resulting in uneven dispersion and reduced mechanical strength and mechanical properties of the material.

[0006] (II) Technical solution

[0007] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a process for preparing alumina composite polishing liquid for diamond substrate, comprising the following formula raw materials in weight proportion: 1-4 parts of polishing liquid, 22-40 parts of diethylene glycol monobutyl ether, 17-22 parts of polycarbonate 1,6-hexanediol ester diol, 20-24 parts of isophorone diisocyanate, 0.5-1 parts of alkylphenol polyoxyethylene ether, 0.5-1 parts of No. 5 white mineral oil, 1-3 parts of No. 10 white mineral oil, 5-7 parts of ethylene glycol monooctyl ether, 15-18 parts of deionized water, and the preparation method includes the following ingredients: hexadecyltrimethylammonium bromide, corrosion inhibitor, silicate, dispersant, suspending agent, surfactant, and alumina particles.

[0008] Preferably, the corrosion inhibitor, silicate, dispersant, suspending agent, surfactant and alumina particles are all of chemical analysis grade.

[0009] Preferably, the polishing liquid introduces functionalized carboxyl groups on the graphene surface and in the pores by a hydrothermal synthesis method, and the preparation method is as follows:

[0010] Add 200 mL of silicate to a 500 mL beaker, weigh 66-78 parts of graphene and 10-14 parts of corrosion inhibitor in turn, and slowly drop 12-20 parts by mass of hexadecyltrimethylammonium bromide. After stirring evenly, transfer the material in the beaker into a reactor for emulsification, and place it in a reactor heating box and heat it to 170-180°C for reaction for 20-24 hours. After the reaction is completed, cool the material to room temperature, filter the solvent to obtain a solid mixture, and wash the solid with 3000-4000 mL of silicate, and place it in an oven and heat it to 90-95°C to dry the water for 3-4 hours to obtain a polishing liquid.

[0011] Preferably, the diethylene glycol monobutyl ether is an amphiphilic copolymer, and the preparation method is as follows:

[0012] Inert gas N2 is introduced into a 2000mL three-necked flask to expel the air, and then 1000mL of silicate is added. 28-35 parts of aluminum oxide particles and 55-68 parts of surfactant are weighed in sequence and added to the three-necked flask. Then 3-7 parts of suspending agent and 1-2 parts of potassium persulfate are slowly added dropwise. The three-necked flask is placed in a constant temperature water bath and heated to 55-60°C. After constant temperature polymerization for 8-10 hours, anhydrous ethanol is slowly added until a large amount of white precipitate is generated. Then the solution is filtered to remove the solvent to obtain a white solid, and the white solid is washed with 500-800mL of anhydrous ethanol, and placed in an oven heated to 90-95°C to dry the water for 5-6 hours to obtain diethylene glycol monobutyl ether.

[0013] Preferably, the alkylphenol polyoxyethylene ether is chemically analytically pure dibutyltin dilaurate.

[0014] Preferably, the No. 5 white mineral oil is a chemically pure malonate.

[0015] Preferably, the No. 10 white mineral oil is chemically analytically pure ammonium persulfate.

[0016] Preferably, the ethylene glycol monooctyl ether is chemically pure hexafluorobutyl acrylate.

[0017] Preferably, the deionized water is chemically pure 2,2-dihydroxymethylbutyric acid.

[0018] Preferably, the polishing liquid is prepared by the following method:

[0019] N2 was introduced into a 2000mL three-necked flask to exhaust the air, and then 800mL of methyl methacrylate was added as a polymerization solvent, and then 17-22 parts of polycarbonate 1,6-hexanediol ester diol, 20-24 parts of isophorone diisocyanate and 15-18 parts of deionized water 2,2-dihydroxymethylbutyric acid were added in sequence, and after stirring evenly, 0.5-1 parts of alkylphenol polyoxyethylene ether dibutyltin dilaurate were added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 85-90°C for reaction for 3-4h, and then 0.5-1 parts of No. 5 white mineral oil malonate were added to double-bond end-cap the prepolymer, and then 20- 30mL of neutralizing agent triethylamine, stir and neutralize for 1-2h, then add 1-3 parts of No. 10 white mineral oil ammonium persulfate and 5-7 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate to the three-necked bottle in sequence, and carry out free radical polymerization for 5-8h. After the reaction, add 1-4 parts of polishing liquid and 22-40 parts of diethylene glycol monobutyl ether to the three-necked bottle, and place the three-necked bottle in an ultrasonic disperser, heat to 70-75°C, the ultrasonic frequency is 20KHz, and ultrasonic treatment is carried out for 2-3h. Then, the three-necked bottle is placed in an oven and heated to 90-95°C, the solvent is slowly evaporated, and the solid-liquid ratio is controlled to be 25-35% to obtain a polishing liquid.

[0020] (III) Beneficial technical effects

[0021] Compared with the prior art, the present invention has the following beneficial technical effects:

[0022] 1. A process for preparing alumina composite polishing liquid for diamond substrates. Polyurethane modified with diethylene glycol monobutyl ether with high chemical energy improves the cleaning effect of the polishing liquid and enhances the production efficiency of the polishing liquid. A large number of fracture structures and micro cracks are formed at the interface between the alumina particle-suspending agent block and the polyurethane. When external stress acts on the polishing liquid, the elastic structure of the fracture structure and the micro crack can absorb the fracture energy generated by the deformation process, inhibiting the secondary expansion of the cracks in the polishing liquid and effectively enhancing the mechanical properties of the polishing liquid, such as toughness and bending strength.

[0023] 2. The process for preparing an alumina composite polishing liquid for diamond substrates introduces functionalized carboxyl groups on graphene, and forms trace ester groups with amino groups on alumina particles in diethylene glycol monobutyl ether through a hydrothermal method, so that diethylene glycol monobutyl ether is uniformly loaded on the surface and inside the pores of graphene, thereby avoiding the agglomeration of diethylene glycol monobutyl ether to form large particle ions due to intermolecular forces, which causes the diethylene glycol monobutyl ether to lose its performance. In addition, the functionalized carboxyl groups form non-metallic covalent bond forces with fluorinated polyurethane, and the three form a three-dimensional network structure with diethylene glycol monobutyl ether, which greatly improves the mechanical properties of the polishing liquid, such as the fracture strength and tensile strength.

[0024] 3. A process for preparing alumina composite polishing liquid for diamond substrates. Diethylene glycol monobutyl ether is an amphiphilic polymer. After forming a copolymer with polyurethane, the polishing liquid has hydrophilic and lipophilic amphiphilic properties. At the same time, the functionalized carboxyl groups on graphene also greatly improve the quality of the polishing liquid. The synergistic effect of the two enhances the practicability and applicability of the polishing liquid in practical applications. DETAILED DESCRIPTION

[0025] To achieve the above-mentioned purpose, the present invention provides the following technical scheme: a process for preparing alumina composite polishing liquid for diamond substrate, comprising the following formula raw materials in weight proportion: 1-4 parts of polishing liquid, 22-40 parts of diethylene glycol monobutyl ether, 17-22 parts of polycarbonate 1,6-hexanediol ester diol, 20-24 parts of isophorone diisocyanate, 0.5-1 parts of alkylphenol polyoxyethylene ether, 0.5-1 parts of No. 5 white mineral oil, 1-3 parts of No. 10 white mineral oil, 5-7 parts of ethylene glycol monooctyl ether, 15-18 parts of deionized water, and the preparation method includes the following ingredients: hexadecyltrimethylammonium bromide, corrosion inhibitor, silicate, dispersant, suspending agent, surfactant, alumina particles

[0026] The corrosion inhibitor, silicate, dispersant, suspending agent, surfactant and alumina particles are all of chemical analysis grade. The polishing liquid introduces functional carboxyl functional groups on the graphene surface and pores by hydrothermal synthesis. The preparation method is as follows:

[0027] Add 200 mL of silicate to a 500 mL beaker, weigh 66-78 parts of graphene and 10-14 parts of corrosion inhibitor in turn, and slowly drop 12-20 parts by mass of hexadecyltrimethylammonium bromide. After stirring evenly, transfer the material in the beaker into a reactor for emulsification, and place it in a reactor heating box and heat it to 170-180°C for reaction for 20-24 hours. After the reaction is completed, cool the material to room temperature, filter the solvent to obtain a solid mixture, and wash the solid with 3000-4000 mL of silicate, and place it in an oven and heat it to 90-95°C to dry the water for 3-4 hours to obtain a polishing liquid.

[0028] Diethylene glycol monobutyl ether is an amphiphilic copolymer, and the preparation method is as follows: inert gas N2 is introduced into a 2000mL three-necked bottle to exhaust the air, and then 1000mL of silicate is added, 28-35 parts of aluminum oxide particles and 55-68 parts of surfactants are weighed in turn and added to the three-necked bottle, and then 3-7 parts of suspending agent and 1-2 parts of potassium persulfate are slowly added dropwise, and the three-necked bottle is placed in a constant temperature water bath and heated to 55-60°C. After constant temperature polymerization for 8-10 hours, anhydrous ethanol is slowly added until a large amount of white precipitate is generated, and then the solution is filtered to remove the solvent to obtain a white solid, and the white solid is washed with 500-800mL of anhydrous ethanol, and placed in an oven heated to 90-95°C to dry the water for 5-6 hours to obtain diethylene glycol monobutyl ether.

[0029] The alkylphenol polyoxyethylene ether is chemically pure dibutyltin dilaurate, No. 5 white mineral oil is chemically pure malonate, No. 10 white mineral oil is chemically pure ammonium persulfate, ethylene glycol monooctyl ether is chemically pure hexafluorobutyl acrylate, deionized water is chemically pure 2,2-dihydroxymethylbutyric acid, and the polishing liquid is prepared as follows:

[0030] N2 was introduced into a 2000mL three-necked flask to exhaust the air, and then 800mL of methyl methacrylate was added as a polymerization solvent, and then 17-22 parts of polycarbonate 1,6-hexanediol ester diol, 20-24 parts of isophorone diisocyanate and 15-18 parts of deionized water 2,2-dihydroxymethylbutyric acid were added in sequence, and after stirring evenly, 0.5-1 parts of alkylphenol polyoxyethylene ether dibutyltin dilaurate were added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 85-90°C for reaction for 3-4h, and then 0.5-1 parts of No. 5 white mineral oil malonate were added to double-bond end-cap the prepolymer, and then 20- 30mL of neutralizing agent triethylamine, stir and neutralize for 1-2h, then add 1-3 parts of No. 10 white mineral oil ammonium persulfate and 5-7 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate to the three-necked bottle in sequence, and carry out free radical polymerization for 5-8h. After the reaction, add 1-4 parts of polishing liquid and 22-40 parts of diethylene glycol monobutyl ether to the three-necked bottle, and place the three-necked bottle in an ultrasonic disperser, heat to 70-75°C, the ultrasonic frequency is 20KHz, and ultrasonic treatment is carried out for 2-3h. Then, the three-necked bottle is placed in an oven and heated to 90-95°C, the solvent is slowly evaporated, and the solid-liquid ratio is controlled to be 25-35% to obtain a polishing liquid.

[0031] Embodiment 1:

[0032] (1) Preparation of polishing liquid: Add 200 mL of silicate into a 500 mL beaker, weigh 78 parts of graphene and 10 parts of corrosion inhibitor in turn, and slowly drop 12 parts by mass of hexadecyltrimethylammonium bromide. After stirring evenly, transfer the materials in the beaker into a reactor for emulsification, and place the materials in the reactor in a heating box and heat them to 170°C for reaction for 24 hours. After the reaction is completed, cool the materials to room temperature, filter the solvent to obtain a solid mixture, wash the solid with 4000 mL of silicate, and place the solid in an oven and heat it to 90°C to dry the water for 4 hours to obtain polishing liquid component 1.

[0033] (2) Preparation of diethylene glycol monobutyl ether as an amphiphilic copolymer: Inert gas N2 was introduced into a 2000 mL three-necked flask to expel the air, and then 1000 mL of silicate was added. 28 parts of alumina particles and 68 parts of surfactant were weighed and added to the three-necked flask in turn. Then 3 parts of suspending agent and 1 part of potassium persulfate were slowly added dropwise. The three-necked flask was placed in a constant temperature water bath and heated to 55°C. After constant temperature polymerization for 8 hours, anhydrous ethanol was slowly added until a large amount of white precipitate was generated. Then, the solution was filtered to remove the solvent to obtain a white solid. The white solid was washed with 500 mL of anhydrous ethanol and placed in an oven heated to 95°C to dry the water for 5 hours to obtain diethylene glycol monobutyl ether component 1.

[0034] (3) Preparation of polishing liquid: N2 was introduced into a 2000 mL three-necked flask to exhaust air, and then 800 mL of methyl methacrylate was added as a polymerization solvent, and then 17 parts of polycarbonate 1,6-hexanediol, 20 parts of isophorone diisocyanate and 15 parts of deionized water 2,2-dihydroxymethylbutyric acid were added in sequence, and after stirring evenly, 0.5 parts of alkylphenol polyoxyethylene ether dibutyltin dilaurate were added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 85°C for reaction for 3 hours, and then 0.5 parts of No. 5 white mineral oil malonate was added to double-bond-cap the prepolymer, and then Add 20 mL of the neutralizing agent triethylamine, stir and neutralize for 1 hour, then add 1 part of No. 10 white mineral oil ammonium persulfate and 5 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate to the three-necked bottle in sequence, and carry out free radical polymerization for 5 hours. After the reaction, add 1 part of polishing liquid component 1 and 40 parts of diethylene glycol monobutyl ether component 1 to the three-necked bottle, and place the three-necked bottle in an ultrasonic disperser, heat to 70°C, the ultrasonic frequency is 20KHz, and ultrasonic treatment is carried out for 2 hours. Then, place the three-necked bottle in an oven and heat to 90°C, slowly evaporate the solvent, and control the solid-liquid ratio to 25% to obtain a polishing liquid product 1.

[0035] Embodiment 2:

[0036] (1) Preparation of polishing liquid: Add 200 mL of silicate into a 500 mL beaker, weigh 75 parts of graphene and 11 parts of corrosion inhibitor in turn, and slowly drop 14 parts of hexadecyltrimethylammonium bromide by mass. After stirring evenly, transfer the materials in the beaker into a reactor for emulsification, and place the materials in the reactor in a heating box and heat them to 170°C for reaction for 20 hours. After the reaction is completed, cool the materials to room temperature, filter the solvent to obtain a solid mixture, wash the solid with 3500 mL of silicate, and place the solid in an oven and heat it to 90°C to dry the water for 3 hours to obtain polishing liquid component 2.

[0037] (2) Preparation of diethylene glycol monobutyl ether as an amphiphilic copolymer: Inert gas N2 was introduced into a 2000 mL three-necked flask to expel the air, and then 1000 mL of silicate was added. 30 parts of alumina particles and 65 parts of surfactant were weighed and added to the three-necked flask in turn. Then 4 parts of suspending agent and 1 part of potassium persulfate were slowly added dropwise. The three-necked flask was placed in a constant temperature water bath and heated to 60°C. After constant temperature polymerization for 8 hours, anhydrous ethanol was slowly added until a large amount of white precipitate was generated. The solution was then filtered to remove the solvent to obtain a white solid. The white solid was washed with 500 mL of anhydrous ethanol and placed in an oven heated to 90°C to dry the water for 6 hours to obtain diethylene glycol monobutyl ether component 2.

[0038] (3) Preparation of polishing liquid: N2 was introduced into a 2000 mL three-necked flask to exhaust air, and then 800 mL of methyl methacrylate was added as a polymerization solvent, and then 18 parts of polycarbonate 1,6-hexanediol, 21 parts of isophorone diisocyanate and 16 parts of deionized water 2,2-dihydroxymethylbutyric acid were added in sequence, and after stirring evenly, 0.6 parts of alkylphenol polyoxyethylene ether dibutyltin dilaurate were added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 90°C for reaction for 3 hours, and then 0.6 parts of No. 5 white mineral oil malonate was added to double-bond-cap the prepolymer, and then 20 mL of neutralizing agent triethylamine, stir and neutralize for 1 hour, then add 1.2 parts of No. 10 white mineral oil ammonium persulfate and 1.2 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate into the three-necked bottle in sequence, and carry out free radical polymerization for 6 hours. After the reaction, add 5.4 parts of polishing liquid component 2 and 36 parts of diethylene glycol monobutyl ether component 2 into the three-necked bottle, and place the three-necked bottle in an ultrasonic disperser, heat to 70°C, ultrasonic frequency of 20KHz, ultrasonic treatment for 2 hours, then place the three-necked bottle in an oven and heat to 90°C, slowly evaporate the solvent, control the solid-liquid ratio to 27%, and obtain polishing liquid product 2.

[0039] Embodiment 3:

[0040] (1) Preparation of polishing liquid: Add 200 mL of silicate into a 500 mL beaker, weigh 72 parts of graphene and 12 parts of corrosion inhibitor in turn, and slowly drop 16 parts of hexadecyltrimethylammonium bromide by mass. After stirring evenly, transfer the materials in the beaker into a reactor for emulsification, and place the materials in the reactor in a heating box and heat to 170°C for reaction for 22 hours. After the reaction is completed, cool the materials to room temperature, filter the solvent to obtain a solid mixture, wash the solid with 3500 mL of silicate, and place the solid in an oven and heat to 90°C to dry the water for 4 hours to obtain polishing liquid component 3.

[0041] (2) Preparation of diethylene glycol monobutyl ether as an amphiphilic copolymer: Inert gas N2 was introduced into a 2000 mL three-necked flask to expel the air, and then 1000 mL of silicate was added. 31.5 parts of alumina particles and 62 parts of surfactant were weighed and added to the three-necked flask in turn. Then 5 parts of suspending agent and 1.5 parts of potassium persulfate were slowly added dropwise. The three-necked flask was placed in a constant temperature water bath and heated to 60°C. After constant temperature polymerization for 10 hours, anhydrous ethanol was slowly added until a large amount of white precipitate was generated. Then, the solution was filtered to remove the solvent to obtain a white solid, and the white solid was washed with 600 mL of anhydrous ethanol, and placed in an oven heated to 95°C to dry the water for 6 hours to obtain diethylene glycol monobutyl ether component 3.

[0042] (3) Preparation of polishing liquid: N2 was introduced into a 2000 mL three-necked flask to exhaust air, and then 800 mL of methyl methacrylate was added as a polymerization solvent, and then 19.5 parts of polycarbonate 1,6-hexanediol, 22 parts of isophorone diisocyanate and 16.5 parts of deionized water 2,2-dimethylolbutyric acid were added in sequence, and after stirring evenly, 0.7 parts of alkylphenol polyoxyethylene ether dibutyltin dilaurate were added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 90°C for reaction for 4 hours, and then 0.8 parts of No. 5 white mineral oil malonate was added to double-bond-cap the prepolymer, and then Add 25 mL of neutralizing agent triethylamine, stir and neutralize for 1 hour, then add 2 parts of No. 10 white mineral oil ammonium persulfate and 6 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate to the three-necked bottle in sequence, and carry out free radical polymerization for 5 hours. After the reaction, add 2.5 parts of polishing liquid component 3 and 30 parts of diethylene glycol monobutyl ether component 3 to the three-necked bottle, and place the three-necked bottle in an ultrasonic disperser, heat to 70°C, the ultrasonic frequency is 20KHz, and ultrasonic treatment is carried out for 3 hours. Then, place the three-necked bottle in an oven and heat to 90°C, slowly evaporate the solvent, control the solid-liquid ratio to 29%, and obtain the polishing liquid product 3.

[0043] Embodiment 4:

[0044] (1) Preparation of polishing liquid: Add 200 mL of silicate into a 500 mL beaker, weigh 69 parts of graphene and 13 parts of corrosion inhibitor in turn, and slowly drop 18 parts of hexadecyltrimethylammonium bromide by mass. After stirring evenly, transfer the material in the beaker into a reactor for emulsification, and place it in a reactor heating box and heat it to 180°C for reaction for 24 hours. After the reaction is completed, cool the material to room temperature, filter the solvent to obtain a solid mixture, and wash the solid with 4000 mL of silicate, and place it in an oven and heat it to 95°C to dry the water for 3 hours to obtain polishing liquid component 4.

[0045] (2) Preparation of diethylene glycol monobutyl ether as an amphiphilic copolymer: Inert gas N2 was introduced into a 2000 mL three-necked flask to expel the air, and then 1000 mL of silicate was added. 33 parts of alumina particles and 59 parts of surfactant were weighed and added to the three-necked flask in turn. Then 6 parts of suspending agent and 2 parts of potassium persulfate were slowly added dropwise. The three-necked flask was placed in a constant temperature water bath and heated to 55°C. After constant temperature polymerization for 10 hours, anhydrous ethanol was slowly added until a large amount of white precipitate was generated. Then, the solution was filtered to remove the solvent to obtain a white solid. The white solid was washed with 800 mL of anhydrous ethanol and placed in an oven heated to 95°C to dry the water for 6 hours to obtain diethylene glycol monobutyl ether component 4.

[0046] (3) Preparation of polishing liquid: N2 was introduced into a 2000 mL three-necked flask to exhaust air, and then 800 mL of methyl methacrylate was added as a polymerization solvent, and then 20 parts of polycarbonate 1,6-hexanediol, 23 parts of isophorone diisocyanate and 17 parts of deionized water 2,2-dimethylolbutyric acid were added in sequence, and after stirring evenly, 0.9 parts of alkylphenol polyoxyethylene ether dibutyltin dilaurate were added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 85°C for 4 hours, and then 0.8 parts of No. 5 white mineral oil malonate was added to double-bond-cap the prepolymer, and then 30 mL of neutralizing agent triethylamine, stir and neutralize for 2 hours, then add 2.7 parts of No. 10 white mineral oil ammonium persulfate and 6.4 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate into the three-necked bottle in sequence, and carry out free radical polymerization for 8 hours. After the reaction, add 3.2 parts of polishing liquid component 4 and 26 parts of diethylene glycol monobutyl ether component 4 into the three-necked bottle, and place the three-necked bottle in an ultrasonic disperser, heat to 75°C, the ultrasonic frequency is 20KHz, and ultrasonic treatment is carried out for 3 hours. Then, the three-necked bottle is placed in an oven and heated to 95°C, the solvent is slowly evaporated, and the solid-liquid ratio is controlled to 32% to obtain a polishing liquid product 4.

[0047] Embodiment 5:

[0048] (1) Preparation of polishing liquid: Add 200 mL of silicate into a 500 mL beaker, weigh 66 parts of graphene and 14 parts of corrosion inhibitor in turn, and slowly drop 20 parts by mass of hexadecyltrimethylammonium bromide. After stirring evenly, transfer the materials in the beaker into a reactor for emulsification, and place the materials in the reactor in a heating box and heat them to 180°C for reaction for 24 hours. After the reaction is completed, cool the materials to room temperature, filter the solvent to obtain a solid mixture, wash the solid with 4000 mL of silicate, and place the solid in an oven and heat it to 95°C to dry the water for 4 hours to obtain polishing liquid component 5.

[0049] (2) Preparation of diethylene glycol monobutyl ether as an amphiphilic copolymer: Inert gas N2 was introduced into a 2000 mL three-necked flask to expel the air, and then 1000 mL of silicate was added. 35 parts of alumina particles and 55 parts of surfactant were weighed and added to the three-necked flask in turn. Then 7 parts of suspending agent and 2 parts of potassium persulfate were slowly added dropwise. The three-necked flask was placed in a constant temperature water bath and heated to 60°C. After constant temperature polymerization for 10 hours, anhydrous ethanol was slowly added until a large amount of white precipitate was generated. The solution was then filtered to remove the solvent to obtain a white solid. The white solid was washed with 800 mL of anhydrous ethanol and placed in an oven heated to 95°C to dry the water for 6 hours to obtain diethylene glycol monobutyl ether component 5.

[0050] (3) Preparation of polishing liquid: N2 was introduced into a 2000 mL three-necked flask to exhaust the air, and then 800 mL of methyl methacrylate was added as a polymerization solvent, and then 22 parts of polycarbonate 1,6-hexanediol, 24 parts of isophorone diisocyanate and 18 parts of deionized water 2,2-dihydroxymethylbutyric acid were added in sequence, and after stirring evenly, 1 part of alkylphenol polyoxyethylene ether dibutyltin dilaurate was added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 90°C for 4 hours, and then 1 part of No. 5 white mineral oil malonate was added to double-bond-cap the prepolymer, and then added 30mL of the neutralizing agent triethylamine was stirred for neutralization for 2h, and then 3 parts of No. 10 white mineral oil ammonium persulfate and 7 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate were added to the three-necked bottle in sequence to carry out free radical polymerization for 8h. After the reaction, 4 parts of the polishing liquid component 5 and 22 parts of diethylene glycol monobutyl ether component 5 were added to the three-necked bottle, and the three-necked bottle was placed in an ultrasonic disperser, heated to 75°C, the ultrasonic frequency was 20KHz, and ultrasonic treatment was performed for 3h. Then the three-necked bottle was placed in an oven and heated to 95°C, the solvent was slowly evaporated, and the solid-liquid ratio was controlled to be 35% to obtain the polishing liquid product 5.

[0051] By performing quality tests, lipophilicity tests, tensile strength tests, fracture strength tests, and toughness tests on Examples 1-5, the preparation process of the alumina composite polishing liquid for diamond substrates, the high chemical energy diethylene glycol monobutyl ether modified polyurethane, improves the cleaning effect of the polishing liquid, enhances the production efficiency of the polishing liquid, and forms a large number of fracture structures and micro cracks at the interface of the alumina particle-suspending agent block and the polyurethane. When external stress acts on the polishing liquid, the elastic structure of the fracture structure and the micro crack can absorb the fracture energy generated by the deformation process, inhibiting the secondary expansion of the cracks in the polishing liquid, and effectively enhancing the mechanical properties of the polishing liquid such as toughness and bending strength. The specific results are shown in Table 1:

[0052] Table 1

[0053] Liquidity Curing temperature Waterproof High temperature resistance Mechanical strength Example 1 0.532m / s 95.7℃ III 165℃ <![CDATA[1275j / cm 2 ]]> Example 2 0.8452m / s 108.4℃ II 134℃ <![CDATA[1143j / cm 2 ]]> Example 3 1.2m / s 112℃ III 137℃ <![CDATA[1386j / cm 2 ]]> Example 4 0.632m / s 94.7℃ III 155℃ <![CDATA[1255j / cm 2 ]]> Example 5 0.5452m / s 104.4℃ II 144℃ <![CDATA[1153j / cm 2 ]]>

[0054] It can be seen from Table 1 that the mechanical properties such as toughness and bending strength of the polishing liquid obtained from the positive unsaturated polyester resin in Examples 1-5 are significantly improved.

[0055] The invention discloses a process for preparing a composite alumina polishing liquid for diamond substrates. Functionalized carboxyl groups are introduced into graphene to form trace ester groups with amino groups on alumina particles in diethylene glycol monobutyl ether through a hydrothermal method, so that diethylene glycol monobutyl ether is uniformly loaded on the surface and inside the pores of graphene, thereby avoiding the formation of large particle ions due to intermolecular forces of diethylene glycol monobutyl ether and causing the loss of performance of diethylene glycol monobutyl ether. Furthermore, the functionalized carboxyl groups form non-metallic covalent bond forces with fluorinated polyurethane, and the three form a three-dimensional network structure with diethylene glycol monobutyl ether, thereby greatly improving the mechanical properties of the polishing liquid, such as the fracture strength and tensile strength.

[0056] The invention discloses a process for preparing alumina composite polishing liquid for diamond substrate. Diethylene glycol monobutyl ether is an amphiphilic polymer. After forming a copolymer with polyurethane, the polishing liquid has the amphiphilic property of hydrophilicity and lipophilicity. Meanwhile, the functionalized carboxyl groups on graphene also greatly improve the quality of the polishing liquid. The synergistic effect of the two enhances the practicability and application range of the polishing liquid in practical applications.

Claims

1. A process for preparing alumina composite polishing liquid for diamond substrate, comprising the following formula raw materials in proportion by weight, characterized in that: 1-4 parts of polishing liquid, 22-40 parts of diethylene glycol monobutyl ether, 17-22 parts of polycarbonate 1,6-hexanediol ester diol, 20-24 parts of isophorone diisocyanate, 0.5-1 parts of alkylphenol polyoxyethylene ether, 0.5-1 parts of No. 5 white mineral oil, 1-3 parts of No. 10 white mineral oil, 5-7 parts of ethylene glycol monooctyl ether, 15-18 parts of deionized water, the preparation method includes the following ingredients: hexadecyltrimethylammonium bromide, corrosion inhibitor, silicate, dispersant, suspending agent, surfactant, aluminum oxide particles.

2. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The corrosion inhibitor, silicate, dispersant, suspending agent, surfactant and alumina particles are all of chemical analysis grade.

3. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The polishing liquid introduces functionalized carboxyl functional groups into the graphene surface and pores by a hydrothermal synthesis method, and the preparation method is as follows: Add 200 mL of silicate to a 500 mL beaker, weigh 66-78 parts of graphene and 10-14 parts of corrosion inhibitor in turn, and slowly drop 12-20 parts by mass of hexadecyltrimethylammonium bromide. After stirring evenly, transfer the material in the beaker into a reactor for emulsification, and place it in a reactor heating box and heat it to 170-180°C for reaction for 20-24 hours. After the reaction is completed, cool the material to room temperature, filter the solvent to obtain a solid mixture, and wash the solid with 3000-4000 mL of silicate, and place it in an oven and heat it to 90-95°C to dry the water for 3-4 hours to obtain a polishing liquid.

4. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The diethylene glycol monobutyl ether is an amphiphilic copolymer, and the preparation method is as follows: Inert gas N2 is introduced into a 2000mL three-necked flask to expel the air, and then 1000mL of silicate is added. 28-35 parts of aluminum oxide particles and 55-68 parts of surfactant are weighed in sequence and added to the three-necked flask. Then 3-7 parts of suspending agent and 1-2 parts of potassium persulfate are slowly added dropwise. The three-necked flask is placed in a constant temperature water bath and heated to 55-60°C. After constant temperature polymerization for 8-10 hours, anhydrous ethanol is slowly added until a large amount of white precipitate is generated. Then the solution is filtered to remove the solvent to obtain a white solid, and the white solid is washed with 500-800mL of anhydrous ethanol, and placed in an oven heated to 90-95°C to dry the water for 5-6 hours to obtain diethylene glycol monobutyl ether.

5. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The alkylphenol polyoxyethylene ether is chemically pure dibutyltin dilaurate.

6. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The No. 5 white mineral oil is a chemical analysis pure malonate.

7. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The No. 10 white mineral oil is chemical analysis pure ammonium persulfate.

8. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The ethylene glycol monooctyl ether is chemical analysis pure hexafluorobutyl acrylate.

9. The process for preparing an alumina composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The deionized water is chemically pure 2,2-dihydroxymethylbutyric acid.

10. The process for preparing an aluminum oxide composite polishing liquid for a diamond substrate according to claim 1, characterized in that: The polishing liquid is prepared as follows: N2 was introduced into a 2000mL three-necked flask to exhaust the air, and then 800mL of methyl methacrylate was added as a polymerization solvent, and then 17-22 parts of polycarbonate 1,6-hexanediol ester diol, 20-24 parts of isophorone diisocyanate and 15-18 parts of deionized water 2,2-dihydroxymethylbutyric acid were added in sequence, and after stirring evenly, 0.5-1 parts of alkylphenol polyoxyethylene ether dibutyltin dilaurate were added in sequence, and the three-necked flask was placed in a constant temperature water bath and heated to 85-90°C for reaction for 3-4h, and then 0.5-1 parts of No. 5 white mineral oil malonate were added to double-bond end-cap the prepolymer, and then 20- 30mL of neutralizing agent triethylamine, stir and neutralize for 1-2h, then add 1-3 parts of No. 10 white mineral oil ammonium persulfate and 5-7 parts of ethylene glycol monooctyl ether hexafluorobutyl acrylate to the three-necked bottle in sequence, and carry out free radical polymerization for 5-8h. After the reaction, add 1-4 parts of polishing liquid and 22-40 parts of diethylene glycol monobutyl ether to the three-necked bottle, and place the three-necked bottle in an ultrasonic disperser, heat to 70-75°C, the ultrasonic frequency is 20KHz, and ultrasonic treatment is carried out for 2-3h. Then, the three-necked bottle is placed in an oven and heated to 90-95°C, the solvent is slowly evaporated, and the solid-liquid ratio is controlled to be 25-35% to obtain a polishing liquid.