CN108034362B - Composite polishing solution and preparation method thereof - Google Patents
Composite polishing solution and preparation method thereof Download PDFInfo
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- CN108034362B CN108034362B CN201810049653.7A CN201810049653A CN108034362B CN 108034362 B CN108034362 B CN 108034362B CN 201810049653 A CN201810049653 A CN 201810049653A CN 108034362 B CN108034362 B CN 108034362B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
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- Organic Chemistry (AREA)
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- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention relates to a composite polishing solution and a preparation method thereof, belonging to the field of precision machining and characterized in that the polishing solution comprises 1 ~% of abrasive particles and 75 ~% of base solution according to mass percentage, wherein the abrasive particles consist of I-grade abrasive particles, II-grade abrasive particles and III-grade abrasive particles, the mass ratio of the I-grade abrasive particles, the II-grade abrasive particles and the III-grade abrasive particles is 1:0.5 ~: 0.5 ~, the average particle size of each grade of abrasive particles is 0.5 ~ micron, the I-grade abrasive particles are larger than the II-grade abrasive particles and larger than the III-grade abrasive particles, and the three abrasive particles are respectively and independently selected from diamond particles, cubic BN particles and SiC particles.
Description
Technical Field
The invention relates to a composite 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 comprising 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.
The composite polishing solution comprises, by mass, 1 ~ 25% of abrasive particles and 75 ~ 99% of base solution, wherein the abrasive particles consist of grade I abrasive particles, grade II abrasive particles and grade III abrasive particles, the mass ratio of the grade I abrasive particles to the grade II abrasive particles to the grade III abrasive particles is 1:0.5 ~ 2:0.5 ~ 5, the average particle size of each grade abrasive particle is 0.5 ~ 50 micrometers, the grade I abrasive particles are larger than the grade II abrasive particles and larger than the grade III abrasive particles, the three abrasive particles are respectively and independently selected from diamond particles, cubic BN particles and SiC particles, and the base solution 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 ~ 7.5.5 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 nanoparticles in the copolymer solution obtained in the step (2) according to the proportion of 0.5 ~ 5g:10mL, ultrasonically dispersing, drying, and drying to obtain SiO2And dispersing the nano particles in a medium solvent according to the mass ratio of the nano particles to the medium solvent of 10:4 ~ 8, and performing ultrasonic dispersion to obtain the base solution for the polishing solution.
The composite polishing solution provided by the invention preferably comprises 1 ~ 25% of abrasive particles and 75 ~ 99% of base solution in percentage by mass.
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 composite polishing solution comprises, by mass, 1 ~ 20% of abrasive particles, 0 ~ 5% of water and 75 ~ 99% of base solution.
Further preferably, the polishing solution consists of, 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 during the addition.
According to the composite polishing solution disclosed by the invention, the particle size range of the grade I abrasive particles is preferably 10 ~ 50 micrometers, the particle size range of the grade II abrasive particles is preferably 2 ~ 20 micrometers, the particle size range of the grade III abrasive particles is preferably 0.5 ~ 5 micrometers, and the particle size of the grade I abrasive particles is larger than that of the grade II abrasive particles.
According to the composite polishing solution, the mass ratio of the grade I abrasive particles to the grade II abrasive particles to the grade III abrasive particles is preferably 1:1 ~ 2 to 2:2 ~ 5.
Further, the mass ratio of the grade I abrasive particles to the grade II abrasive particles to the grade III abrasive particles is 1:1.7: 3.3.
In the preparation method of the base solution for the polishing solution, in the step (1), SiO is added2The method comprises the steps of mixing the nano particles, the silane coupling agent and the ethylene glycol according to the mass ratio of 100:1 ~ 2:5 ~ 10, and then carrying out ball milling, wherein the ball milling rotation speed is preferably 800 ~ 2000r/min, and the ball milling time is preferably 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 was 50nm ~ 200nm further, the SiO2The nano particles are preferably nano microspheres, and the average particle size of the nano particles is 80nm ~ 120 nm.
Preferably, in the step (1), the drying is spray drying, and the conditions are that the inlet temperature is 200 ~ 220 ℃, the outlet temperature is 70 ~ 100 ℃, and the pressure of compressed air is 0.5 ~ 1 Mpa.
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.
The preparation method of the base liquid for the polishing liquid comprises the steps of (2) adding ammonium persulfate and acrylic acid into a maleic anhydride aqueous solution in batches at 90-105 ℃, reacting for 4 ~ 6 hours, continuously dropwise adding a NaOH solution in the whole reaction process until the reaction is finished, and adjusting the pH value of the solution to be 7 ~ 7.5.5 after the reaction is finished to obtain a copolymer solution, wherein the molar ratio of maleic anhydride to acrylic acid is 1:0.5 ~ 2, and the molar ratio of ammonium persulfate to 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 maleic anhydride to acrylic acid is 1:1 ~ 1.5.5.
Preferably, the molar ratio of ammonium persulfate to maleic anhydride is 0.5 ~ 2.7.7: 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, the average molecular weight of the polyethylene glycol is 200 ~ 2000, and further preferably, the medium solvent is PEG200, PEG400, PEG600, PEG1000 and 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 had a good dispersion state in the medium solvent and a viscosity of 2 ~ 20Pa · 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 base solution, wherein the abrasive particles comprise three grades of abrasive particles, and the abrasive particles have different average grain diameters and can effectively remove protrusions with different degrees on the surface of a material.
Detailed Description
The base liquid used in the following examples was prepared as follows:
(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 the aqueous solution of the maleic anhydride in batches at 100-105 ℃ simultaneously, reacting for 5 hours, continuously dropwise adding 35% by mass of NaOH solution in the whole reaction process until the reaction is finished, and adjusting the pH value of the solution to be 7 ~ 7.5.5 after the reaction is finished to obtain a copolymer solution, wherein the molar ratio of the maleic anhydride to the acrylic acid is 1: 1.5, and the molar ratio of the ammonium persulfate to the 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 liquid for the polishing solution.
The base liquid for polishing liquid obtained by the method has shear thickening property, SiO2Nano meterThe particles had a good dispersion state in the medium solvent and the viscosity thereof was 5.79 pas.
SiO used2The nano particles are silicon dioxide nano microspheres with the average particle size of 100nm, the silane coupling agent is a silane coupling agent KH570, the drying method is spray drying, the conditions are that the inlet temperature is 210 ~ 215 ℃, the outlet temperature is 85 ~ 90 ℃, the compressed air pressure is 1Mpa, and the medium solvent is PEG 2000.
Example 1 ~ 4
Preparing polishing solution, adding abrasive particles and water (if needed) into base solution in batches, continuously performing ultrasonic dispersion during the adding, wherein the average particle size of the grade I abrasive particles is 20 micrometers, the average particle size of the grade II abrasive particles is 5 micrometers, and the average particle size of the grade III abrasive particles is 2 micrometers, so as to obtain polishing solution 1 ~ 4, respectively placing the polishing solution 1 ~ 4 into a shear thickening polishing device, polishing an alumina ceramic curved workpiece, clamping the alumina ceramic curved workpiece by using a clamp to immerse the alumina ceramic curved workpiece into the polishing solution in a liquid tank, fixing the liquid tank, rotating the clamp at a rotating speed of 100r/min for 30min, wherein the surface roughness Ra of the alumina ceramic curved workpiece before treatment is 129.6nm, and the results after the polishing treatment are shown in the following table 1:
comparative example 1
And (3) preparing a polishing solution, adding abrasive particles into the base solution in batches, and continuously performing ultrasonic dispersion during the adding process, wherein the average particle size of the abrasive particles is 5 micrometers.
TABLE 1
The content of each raw material component is the percentage of the total mass of the polishing solution.
Claims (10)
1. The composite polishing solution is characterized by comprising, by mass, 1 ~ 25% of abrasive particles and 75 ~ 99% of base solution, wherein the abrasive particles consist of grade I abrasive particles, grade II abrasive particles and grade III abrasive particles, the mass ratio of the grade I abrasive particles to the grade II abrasive particles to the grade III abrasive particles is 1:0.5 ~ 2:0.5 ~ 5, the average particle size of each grade abrasive particle is 0.5 ~ 50 micrometers, the grade I abrasive particles are larger than the grade II abrasive particles and larger than the grade III abrasive particles, the three abrasive particles are respectively and independently selected from diamond particles, CBN particles and SiC particles, and the base solution 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 ~ 7.5.5 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 nanoparticles in the copolymer solution obtained in the step (2) according to the proportion of 0.5 ~ 5g:10mL, ultrasonically dispersing, drying, and drying to obtain SiO2And dispersing the nano particles in a medium solvent according to the mass ratio of the nano particles to the medium solvent of 10:4 ~ 8, and performing ultrasonic dispersion to obtain the base solution for the polishing solution.
2. The polishing solution according to claim 1, wherein in the step (1), the SiO is2The average particle diameter of the nanoparticles was 50nm ~ 200 nm.
3. The polishing solution according to claim 1, wherein in the step (1), the ball milling rotation speed is 800 ~ 2000 r/min.
4. The polishing solution of claim 1, wherein in the step (2), the mass ratio of the maleic anhydride to the water is 28 ~ 35: 100.
5. The polishing solution according to claim 1, wherein in the step (2), the molar ratio of maleic anhydride to acrylic acid is 1:1 ~ 1.5.5, and the molar ratio of ammonium persulfate to maleic anhydride is 0.5 ~ 2.7.7: 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 ~ 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 grade I abrasive particles have a particle size range of 10 ~ 50 microns, the grade II abrasive particles have a particle size range of 2 ~ 20 microns, and the grade III abrasive particles have a particle size range of 0.5 ~ 5 microns.
10. The polishing solution according to claim 1, wherein the polishing solution comprises, by mass, 1 ~ 25% of abrasive grains and 75 ~ 99% of a base solution.
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| CN109760218B (en) * | 2019-02-18 | 2021-06-08 | 郑君雄 | Preparation method of ultra-precise semiconductor material for electronics and communication industries |
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