CN108178987B - Polishing solution and preparation method thereof - Google Patents
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- CN108178987B CN108178987B CN201810049654.1A CN201810049654A CN108178987B CN 108178987 B CN108178987 B CN 108178987B CN 201810049654 A CN201810049654 A CN 201810049654A CN 108178987 B CN108178987 B CN 108178987B
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Abstract
The invention relates to a polishing solution and a preparation method thereof, belonging to the field of precision machining. The polishing solution comprises, by mass, 1-25% of abrasive particles and 75-99% of a base solution, wherein the abrasive particles are diamond particles with an average particle size of 0.5-50 micrometers. The preparation method of the base liquid comprises the following process steps: mixing SiO2Pretreating the nano particles; preparing a copolymer solution, pretreating the obtained SiO2Dissolving the nano particles in the copolymer solution obtained in the step, and performing ultrasonic dispersion and drying; drying the obtained SiO2Dispersing the nano particles in a medium solvent according to the mass ratio of 10: 4-8, and performing ultrasonic dispersion to obtain the base liquid for the polishing solution. The polishing solution ensures that the silicon dioxide nanoparticles have good dispersibility in the preparation process, and ensures the polishing effect and speed due to the formation of nanoparticle particle clusters in the polishing solution when the non-Newtonian fluid is used for polishing.
Description
Technical Field
The invention relates to a polishing solution and a preparation method thereof, belonging to the field of precision machining.
Background
Currently, commonly used polishing methods include chemical polishing, mechanical polishing, electrolytic polishing, ultrasonic polishing, magnetic grinding polishing, chemical mechanical polishing, etc., wherein some methods, such as mechanical polishing and chemical mechanical polishing, are only suitable for planar planarization polishing, but not for polishing curved workpieces due to the limitation of their polishing methods. Other polishing methods that can be used for curved surfaces have problems. Such as magnetic grinding and polishing, the polishing method is to form an abrasive brush by using magnetic abrasive under the action of a magnetic field and grind and process a workpiece. The method has high processing efficiency, good quality, easy control of processing conditions and good working conditions, but needs to be exchanged into a complex magnetic field generating device and a control system, and has high cost and energy consumption. As another example, the basic principle of electropolishing is the same as chemical polishing, i.e., the surface is made smooth by selectively dissolving the tiny protrusions on the surface of the material. Compared with chemical polishing, the method can eliminate the influence of cathode reaction and has better effect. However, most of the electrolyte is corrosive liquid, which is easy to cause pollution.
Polishing by utilizing the shear thickening property of the non-Newtonian fluid is an emerging polishing means at present, and the polishing is carried out on the surface of a workpiece by utilizing the shear thickening property of the non-Newtonian fluid and abrasive particles. The common non-Newtonian fluid is a non-Newtonian fluid with high viscosity formed by dissolving nano silica particles in a small amount of polymer, and the preparation of the non-Newtonian fluid generally needs multiple dispersing, drying, redispersing and drying processes, and the method has complex process and low success rate. The reason is that the nano particles have high specific surface area and surface activity and are easy to agglomerate. In order to avoid agglomeration of the silica nanoparticles, the silica nanoparticles may be surface-modified, and although the modified silica nanoparticles may be well dispersed in the polymer, they may hinder the formation of particle clusters and reduce the polishing effect and rate.
Disclosure of Invention
In order to solve the above technical problems, an object of the present invention is to provide a polishing liquid including a shear thickening fluid base and abrasive grains. The polishing solution is suitable for polishing workpieces with various surface shapes, and is particularly suitable for polishing the surfaces of curved workpieces. The base liquid has no corrosiveness, has very good shear thickening property, and is suitable for surface processing of metal and ceramic workpieces.
A polishing solution comprises, by mass, 1-25% of abrasive particles and 75-99% of a base solution, wherein the abrasive particles are diamond particles having an average particle size of 0.5-50 μm,
the base liquid is prepared by the following method, and comprises the following process steps:
(1) mixing SiO2Mixing the nano particles, a silane coupling agent and ethylene glycol according to a mass ratio of 100: 1-2: 5-10, performing ball milling for at least 0.5h, and drying after ball milling to obtain pretreated SiO2Nanoparticles;
(2) dissolving maleic anhydride and water in a mass ratio of 15-50: 100 in water, reacting the maleic anhydride and acrylic acid for 4-6 hours at 90-105 ℃ in the presence of ammonium persulfate, dropwise adding a NaOH solution with the mass fraction of 30-40% into a reaction liquid during the reaction, and adjusting the pH value of the solution to 7-7.5 after the reaction is finished to obtain a copolymer solution, wherein the molar ratio of the maleic anhydride to the acrylic acid is 1: 0.5-2, and the molar ratio of the ammonium persulfate to the maleic anhydride is 0.1-5: 100;
(3) the pretreated SiO obtained in the step (1) is treated2The nano particles are dissolved in the solution according to the proportion of 0.5-5 g:10mLCarrying out ultrasonic dispersion and drying on the copolymer solution obtained in the step (2); drying the obtained SiO2Dispersing the nano particles in a medium solvent according to the mass ratio of 10: 4-8, and performing ultrasonic dispersion to obtain the base liquid for the polishing solution.
The polishing solution disclosed by the invention is preferably composed of 1-25% of abrasive particles and 75-99% of base solution by mass percent.
The polishing solution in the technical scheme is prepared by the following method: the abrasive grains are added to the base liquid in portions, and ultrasonic dispersion is continuously performed during the addition.
According to another preferable scheme, the polishing solution comprises, by mass, 1-20% of abrasive particles, 0-5% of water and 75-99% of a base solution.
Preferably, the polishing solution comprises, by mass, 1-20% of abrasive particles, 3-5% of water and 75-96% of a base solution.
The polishing solution in the technical scheme is prepared by the following method: and adding the abrasive particles and water into the base liquid in batches, and continuously performing ultrasonic dispersion in the adding process.
In the preparation method of the base solution for the polishing solution, in the step (1), SiO is added2Mixing the nano particles, the silane coupling agent and the ethylene glycol according to a mass ratio of 100: 1-2: 5-10, and then carrying out ball milling. Further, the ball milling rotating speed is preferably 800-2000 r/min; preferably, the ball milling time is 0.5-2 h.
In the method for preparing the base liquid for polishing slurry according to the present invention, it is preferable that in the step (1), the SiO is2The average particle diameter of the nanoparticles is 50nm to 200 nm. Further, the SiO2The nano particles are preferably nano microspheres, and the average particle size of the nano particles is 80 nm-120 nm.
According to the preparation method of the base solution for the polishing solution, in the step (1), spray drying is preferably adopted, and the conditions of the inlet temperature of 200-220 ℃, the outlet temperature of 70-100 ℃ and the pressure of compressed air of 0.5-1 Mpa are adopted.
In the step (2), maleic anhydride and water are mixed according to a mass ratio of 15-50: 100 at 60-70 ℃ to dissolve the maleic anhydride in the water.
In the step (2), ammonium persulfate and acrylic acid are added into a maleic anhydride aqueous solution in batches at 90-105 ℃, the reaction is carried out for 4-6 hours, and a NaOH solution is continuously dripped in the whole reaction process until the reaction is finished; and after the reaction is finished, adjusting the pH value of the solution to 7-7.5 to obtain a copolymer solution, wherein the molar ratio of the maleic anhydride to the acrylic acid is 1: 0.5-2, and the molar ratio of the ammonium persulfate to the maleic anhydride is 0.1-5: 100.
The copolymer solution obtained by the method in the step (2) is a transparent solution which is a maleic anhydride-acrylic acid copolymer sodium salt solution.
Preferably, in the step (2), the mass ratio of the maleic anhydride to the water is 28-35: 100.
Preferably, the molar ratio of the maleic anhydride to the acrylic acid is 1: 1-1.5.
Preferably, the molar ratio of the ammonium persulfate to the maleic anhydride is 0.5-2.7: 100.
Preferably, in the step (3), the medium solvent is at least one of polyethylene glycol, ethylene glycol and glycerol. Further preferably, the medium solvent is polyethylene glycol, and the average molecular weight of the polyethylene glycol is 200-2000; further preferably, the medium solvent is PEG200, PEG400, PEG600, PEG1000, PEG 2000.
Preferably, the silane coupling agent is one of a silane coupling agent KH570, a silane coupling agent KH-560 and a silane coupling agent Si 69.
The polishing base liquid prepared by the method has shear thickening property and SiO2The nanoparticles have a good dispersion state in a medium solvent, and the viscosity of the nanoparticles is 2-20 Pa & S.
Compared with the prior art, the invention has the advantages that:
the polishing solution comprises, by mass, 1-25% of abrasive particles and 75-99% of a base solution, wherein the abrasive particles are diamond particles with an average particle size of 0.5-50 micrometers. The base liquid used in the invention is non-Newtonian fluid, compared with the non-Newtonian fluid provided by the prior art, the preparation method comprises two modification processes, on one hand, the silicon dioxide nano particles have good dispersibility in the preparation process, and on the other hand, when the non-Newtonian fluid is used for polishing, nano particle clusters are formed in the polishing liquid, and the polishing effect and the polishing speed are ensured.
Detailed Description
SiO used in the following examples 1 to 42The nano particles are silicon dioxide nano microspheres, and the average particle size is 100 nm. The silane coupling agent is a silane coupling agent KH 570.
The drying method used in the following examples 2 to 4 is spray drying, and the conditions are that the inlet temperature is 210 to 215 ℃, the outlet temperature is 85 to 90 ℃, and the pressure of compressed air is 1 Mpa.
The medium solvent used in the following examples 1 and 2 was PEG 400; the medium solvent used in said examples 3 and 4 was PEG 2000.
Example 1
(1) Mixing SiO2Mixing the nano particles, a silane coupling agent and ethylene glycol according to a mass ratio of 100:1.5:8.5, performing ball milling for 0.5h at a ball milling rotation speed of 1200r/min, and performing vacuum drying to obtain pretreated SiO2Nanoparticles;
(2) mixing maleic anhydride and water according to a mass ratio of 30:100 at 60-70 ℃ to dissolve the maleic anhydride in the water; adding ammonium persulfate and acrylic acid into a maleic anhydride aqueous solution in batches at 100-105 ℃, reacting for 5 hours, and continuously dropwise adding a NaOH solution with the mass fraction of 30% in the whole reaction process until the reaction is finished; and after the reaction is finished, adjusting the pH value of the solution to 7-7.5 to obtain a copolymer solution, wherein the molar ratio of the maleic anhydride to the acrylic acid is 1: 2, and the molar ratio of the ammonium persulfate to the maleic anhydride is 2: 100. (ii) a
(3) The pretreated SiO obtained in the step (1) is treated2Dissolving the nano particles in the copolymer solution obtained in the step (2) according to the proportion of 4g:10mL, and performing ultrasonic dispersion and drying; drying the obtained SiO2Dispersing the nano particles in a medium solvent according to the mass ratio of 10:8 of the nano particles to the medium solvent, and performing ultrasonic dispersion to obtain the base liquid for the polishing solution.
The base liquid for polishing liquid obtained by the method has shear thickening property, SiO2The nanoparticles had a good dispersion state in the medium solvent, a viscosity of 3.12 pas, and a viscosity rise of 7.23 pas under a shear stress of 50 Pa.
Example 2
(1) Mixing SiO2Mixing the nano particles, a silane coupling agent and ethylene glycol according to a mass ratio of 100:5:5, performing ball milling for 0.5h at a ball milling rotation speed of 1200r/min, and drying to obtain pretreated SiO2Nanoparticles;
(2) mixing maleic anhydride and water according to the mass ratio of 35:100 at the temperature of 60-70 ℃ to dissolve the maleic anhydride in the water; adding ammonium persulfate and acrylic acid into a maleic anhydride aqueous solution in batches at 100-105 ℃, reacting for 5 hours, and continuously dropwise adding a 35% NaOH solution in the whole reaction process until the reaction is finished; after the reaction is finished, adjusting the pH value of the solution to 7-7.5 to obtain a copolymer solution, wherein the molar ratio of maleic anhydride to acrylic acid is 1: 2, and the molar ratio of ammonium persulfate to maleic anhydride is 3: 100;
(3) the pretreated SiO obtained in the step (1) is treated2Dissolving the nano particles in the copolymer solution obtained in the step (2) according to the proportion of 5g to 10mL, and performing ultrasonic dispersion and drying; drying the obtained SiO2Dispersing the nano particles in a medium solvent according to the mass ratio of the nano particles to the medium solvent of 10:7, and performing ultrasonic dispersion to obtain the base solution for the polishing solution.
The base liquid for polishing liquid obtained by the method has shear thickening property, SiO2The nanoparticles had a good dispersion state in the medium solvent, a viscosity of 4.61 pas, and a viscosity rise of 10.05 pas under a shear stress of 50 Pa.
Example 3
(1) Mixing SiO2Mixing the nano particles, a silane coupling agent and ethylene glycol according to a mass ratio of 100:2:8, performing ball milling for 0.5h at a ball milling rotation speed of 1200r/min, and drying to obtain pretreated SiO2Nanoparticles;
(2) mixing maleic anhydride and water according to a mass ratio of 28:100 at 60-70 ℃ to dissolve the maleic anhydride in the water; adding ammonium persulfate and acrylic acid into a maleic anhydride aqueous solution in batches at 100-105 ℃, reacting for 5 hours, and continuously dropwise adding a 35% NaOH solution in the whole reaction process until the reaction is finished; after the reaction is finished, adjusting the pH value of the solution to 7-7.5 to obtain a copolymer solution, wherein the molar ratio of maleic anhydride to acrylic acid is 1: 1.5, and the molar ratio of ammonium persulfate to maleic anhydride is 2: 100;
(3) the pretreated SiO obtained in the step (1) is treated2Dissolving the nano particles in the copolymer solution obtained in the step (2) according to the proportion of 5g to 10mL, and performing ultrasonic dispersion and drying; drying the obtained SiO2Dispersing the nano particles in a medium solvent according to the mass ratio of the nano particles to the medium solvent of 10:6, and performing ultrasonic dispersion to obtain the base solution for the polishing solution.
The base liquid for polishing liquid obtained by the method has shear thickening property, SiO2The nanoparticles had a good dispersion state in the medium solvent and a viscosity of 5.79 pas.
Example 4
(1) Mixing SiO2Mixing the nano particles, a silane coupling agent and ethylene glycol according to a mass ratio of 100:5:5, then carrying out ball milling for 1h at a ball milling rotation speed of 1200r/min, and drying after ball milling to obtain pretreated SiO2Nanoparticles;
(2) mixing maleic anhydride and water according to the mass ratio of 35:100 at the temperature of 60-70 ℃ to dissolve the maleic anhydride in the water; adding ammonium persulfate and acrylic acid into a maleic anhydride aqueous solution in batches at 100-105 ℃, reacting for 5 hours, and continuously dropwise adding a 35% NaOH solution in the whole reaction process until the reaction is finished; after the reaction is finished, adjusting the pH value of the solution to 7-7.5 to obtain a copolymer solution, wherein the molar ratio of maleic anhydride to acrylic acid is 1: 2, and the molar ratio of ammonium persulfate to maleic anhydride is 3: 100;
(3) the pretreated SiO obtained in the step (1) is treated2Dissolving the nano particles in the copolymer solution obtained in the step (2) according to the proportion of 5g to 10mL, and performing ultrasonic dispersion and drying; drying the obtained SiO2The nanoparticles are in a mass ratio to the medium solventDispersing the mixture in a medium solvent at a ratio of 10:4, and performing ultrasonic dispersion to obtain the base liquid for the polishing solution.
The base liquid for polishing liquid obtained by the method has shear thickening property, SiO2The nanoparticles had a good dispersion state in the medium solvent and a viscosity of 8.46 pas.
Application examples 1 to 4
Preparing polishing solution, adding abrasive particles into base solution in batches, and continuously performing ultrasonic dispersion in the adding process, wherein the polishing solution consists of 12% of abrasive particles and 88% of base solution, the abrasive particles are diamond particles with the average particle size of 10 micrometers, and the base solution is the base solution obtained in example 1 or 2, so that polishing solutions 1 and 2 are obtained.
Preparing polishing solution, adding abrasive particles and water into base solution in batches, and continuously performing ultrasonic dispersion in the adding process, wherein the polishing solution consists of 10% of abrasive particles, 5% of water and 85% of base solution, the abrasive particles are diamond particles with the average particle size of 10 micrometers, and the base solution is the base solution obtained in example 3 or 4, so that polishing solutions 3 and 4 are obtained.
Respectively placing polishing solutions 1-4 in a shearing thickening polishing device, polishing an aluminum oxide ceramic curved surface workpiece, clamping the aluminum oxide ceramic curved surface workpiece by using a clamp to immerse the aluminum oxide ceramic curved surface workpiece into the polishing solution in a liquid tank, fixing the liquid tank, rotating the clamp at a rotating speed of 100r/min, and processing for 30min, wherein the surface roughness Ra of the aluminum oxide ceramic curved surface workpiece before processing is 81.3nm, and the results after polishing are shown in the following table 1:
TABLE 1
| Application example | Application example 1 | Application example 2 | Application example 3 | Application example 4 |
| Surface roughness Ra/nm | 13.2 | 11.9 | 8.2 | 9.8 |
Claims (9)
1. A polishing solution is characterized by comprising 1-25% of abrasive particles and 75-99% of base solution by mass, wherein the abrasive particles are diamond particles with the average particle size of 0.5-50 microns,
the base liquid is prepared by the following method, and comprises the following process steps:
(1) mixing SiO2Mixing the nano particles, a silane coupling agent and ethylene glycol according to a mass ratio of 100: 1-2: 5-10, performing ball milling for at least 0.5h, and drying after ball milling to obtain pretreated SiO2Nanoparticles;
(2) dissolving maleic anhydride and water in a mass ratio of 15-50: 100 in water, reacting the maleic anhydride and acrylic acid for 4-6 hours at 90-105 ℃ in the presence of ammonium persulfate, dropwise adding a NaOH solution with the mass fraction of 30-40% into a reaction liquid during the reaction, and adjusting the pH value of the solution to 7-7.5 after the reaction is finished to obtain a copolymer solution, wherein the molar ratio of the maleic anhydride to the acrylic acid is 1: 0.5-2, and the molar ratio of the ammonium persulfate to the maleic anhydride is 0.1-5: 100;
(3) the pretreated SiO obtained in the step (1) is treated2Dissolving 0.5-5 g of nanoparticles in 10mL of the copolymer solution obtained in the step (2), and performing ultrasonic dispersion and drying; drying the obtained SiO2Dispersing the nano particles in a medium solvent according to the mass ratio of 10: 4-8, and performing ultrasonic dispersion to obtain the base liquid for the polishing solution.
2. Root of herbaceous plantThe polishing solution according to claim 1, wherein in the step (1), the SiO is2The average particle diameter of the nanoparticles is 50nm to 200 nm.
3. The polishing solution according to claim 1, wherein in the step (1), the ball milling rotation speed is 800 to 2000 r/min.
4. The polishing solution according to claim 1, wherein in the step (2), the mass ratio of the maleic anhydride to the water is 28 to 35: 100.
5. The polishing solution according to claim 1, wherein in the step (2), the molar ratio of the maleic anhydride to the acrylic acid is 1:1 to 1.5; the molar ratio of the ammonium persulfate to the maleic anhydride is 0.5-2.7: 100.
6. The polishing solution according to claim 1, wherein in the step (3), the medium solvent is at least one of polyethylene glycol, ethylene glycol and glycerol.
7. The polishing solution according to claim 6, wherein the polyethylene glycol has an average molecular weight of 200 to 2000.
8. The polishing solution according to claim 1, wherein the silane coupling agent is one of a silane coupling agent KH570, a silane coupling agent KH-560, and a silane coupling agent Si 69.
9. The polishing solution according to claim 1, wherein the polishing solution comprises 1 to 25% by mass of abrasive grains and 75 to 99% by mass of a base solution.
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| CN111266938B (en) * | 2020-03-26 | 2021-11-12 | 平湖市鼎天机械有限责任公司 | Workpiece polishing method |
| CN115093829A (en) * | 2022-07-11 | 2022-09-23 | 浙江奥首材料科技有限公司 | Mixed abrasive, optical quartz glass polishing solution containing same, preparation method and application |
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