CN108034363B - Combined polishing solution - Google Patents

Combined polishing solution Download PDF

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Publication number
CN108034363B
CN108034363B CN201810050807.4A CN201810050807A CN108034363B CN 108034363 B CN108034363 B CN 108034363B CN 201810050807 A CN201810050807 A CN 201810050807A CN 108034363 B CN108034363 B CN 108034363B
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polishing
polishing solution
solution
abrasive
maleic anhydride
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CN108034363A (en
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蒋秋菊
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Jiangsu Xiubo New Material Co., Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09GPOLISHING COMPOSITIONS; SKI WAXES
    • C09G1/00Polishing compositions
    • C09G1/02Polishing compositions containing abrasives or grinding agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24BMACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B31/00Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor
    • B24B31/10Machines or devices designed for polishing or abrading surfaces on work by means of tumbling apparatus or other apparatus in which the work and/or the abrasive material is loose; Accessories therefor involving other means for tumbling of work
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00Materials not provided for elsewhere
    • C09K3/14Anti-slip materials; Abrasives
    • C09K3/1409Abrasive particles per se

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Mechanical Treatment Of Semiconductor (AREA)

Abstract

The invention relates to a combined polishing solution, and belongs to the field of precision machining. A combined polishing solution is characterized by comprising two groups of independent polishing solutions I and II, wherein each group of polishing solution comprises 1-25% of abrasive and 75-99% of base solution by mass percent, and the abrasive used by the polishing solution I is alumina whisker, SiC whisker, ZnO whisker and carbon fiber; the grinding material used by the polishing solution II is superhard material particles with the average particle size of 0.5-50 microns. When the combined polishing solution is used for polishing, the polishing solution I is used for polishing firstly, and then the polishing solution II is used for polishing. The abrasive in the polishing solution I is a whisker which can be taken out higher like a 'knife edge' and has a raised material surface; and then, polishing for the second time by using polishing solution II, and treating the surface by using finer abrasive particles. The bulges with different degrees on the surface of the material can be effectively removed by the above method.

Description

Combined polishing solution
Technical Field
The invention relates to a combined polishing solution, and belongs 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, the present invention provides a combined polishing solution, which comprises two separate groups of polishing solutions, wherein the two groups of polishing solutions are used in combination, and each group of polishing solutions comprises a shear thickening fluid base solution and an abrasive. 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 combined polishing solution comprises two groups of independent polishing solutions I and II, wherein each group of polishing solution comprises 1-25% of abrasive and 75-99% of base solution by mass percent, the abrasive used by the polishing solution I is alumina whisker, SiC whisker, ZnO whisker and carbon fiber, the length-diameter ratio of the abrasive is 2-10, and the length of the abrasive is 5-10 micrometers; the grinding material used by the polishing solution II is superhard material particles with the average particle size of 0.5-50 microns, the superhard material is diamond particles, cubic BN particles or SiC particles,
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 treated2NanoparticlesDissolving 0.5-5 g of 10mL of the aqueous solution in 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.
The composite polishing solution disclosed by the invention preferably comprises 1-25% of abrasive particles and 75-99% of base solution by mass percent.
The polishing solution I or II 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 I or II comprises, by mass, 1-20% of abrasive particles, 0-5% of water and 75-99% of 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 during the addition.
In the polishing solution I, the length-diameter ratio of the abrasive is preferably 2-6, and the length of the abrasive is preferably 5-10 micrometers.
In the invention, the grinding material used by the polishing solution II is preferably superhard material particles with the average particle size of 10-20 microns.
The invention further provides a method for polishing a workpiece by using the combined polishing solution I and the combined polishing solution II.
A workpiece polishing method comprises the steps of clamping a workpiece by using a clamp, immersing the surface to be processed of the workpiece into polishing liquid I, controlling the workpiece to rotate at a rotating speed of 20-200 r/min, controlling a liquid tank containing the polishing liquid to rotate in the direction opposite to that of the workpiece at a rotating speed of 0-1000 r/min, and processing for 10-60 min; taking out the workpiece, cleaning and drying; then, immersing the surface to be processed of the workpiece into the polishing solution II, controlling the workpiece to rotate at a rotating speed of 20-200 r/min, controlling a liquid tank containing the polishing solution to rotate in a direction opposite to the workpiece at a rotating speed of 0-1000 r/min, and processing for 10-60 min, cleaning and drying.
In the above technical solution, the method can be performed in commercial shear thickening polishing equipment, and also can be performed in equipment disclosed in the prior art, such as a shear thickening polishing apparatus disclosed in chinese patent publication No. CN 102717325B.
In the above technical scheme, the liquid tank can be fixed.
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 combined polishing solution disclosed by the invention consists of polishing solutions I and II, and each polishing solution comprises 1-25% of abrasive particles and 75-99% of base solution by mass. When the combined polishing solution is used for polishing, the polishing solution I is used for polishing firstly, and then the polishing solution II is used for polishing. The abrasive in the polishing solution I is a whisker which can be taken out higher like a 'knife edge' and has a raised material surface; and then, polishing for the second time by using polishing solution II, and treating the surface by using finer abrasive particles. The bulges with different degrees on the surface of the material can be effectively removed by the above method. 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
The scope of the invention is not limited to the disclosure of the above embodiments, and simple modifications and combinations of the embodiments are within the scope of the invention.
The base solutions used in the following examples 1 to 4 were prepared as follows:
(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 10:7, 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 4.61 pas, and a viscosity rise of 10.05 pas under a shear stress of 50 Pa.
SiO used2The 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 is spray drying, and the conditions are that the inlet temperature is 210-215 ℃, the outlet temperature is 85-90 ℃, and the pressure of compressed air is 1 Mpa; the medium solvent used was PEG 400.
The base solutions used in the following examples 5 to 8 were 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 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 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 5.79 pas.
SiO used2The 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 is spray drying, and the conditions are that the inlet temperature is 210-215 ℃, the outlet temperature is 85-90 ℃, and the pressure of compressed air is 1 Mpa; the medium solvent used was PEG 2000.
Examples 1 to 8
And (3) preparing a polishing solution, adding abrasive particles and water (if needed) into the base solution in batches, and continuously performing ultrasonic dispersion during adding to obtain the combined polishing solution 1-8. And respectively putting the polishing solutions 1-8 into shearing thickening polishing equipment to polish the aluminum oxide ceramic curved surface workpiece.
In examples 1 to 4, the alumina ceramic curved surface workpiece was held by a jig and immersed in the polishing liquid in a liquid bath, and the liquid bath was fixed, and the jig was rotated at a rotation speed of 50r/min and the liquid bath was rotated at a rotation speed of 200rr/min, for 10 minutes each. The polishing solution I uses SiC whiskers as abrasive materials, the length-diameter ratio of the abrasive materials is 2-5, and the length of the abrasive materials is 5-10 micrometers; the abrasive used by the polishing solution II is diamond particles with the average particle size of 10 microns.
In examples 5 to 8, the alumina ceramic curved surface workpiece was held by a jig and immersed in the polishing liquid in a liquid bath, the liquid bath was fixed, and the jig was rotated at a rotation speed of 200r/min, and the liquid bath was fixed, and each treatment was carried out for 15 min. The polishing solution I uses SiC whiskers as abrasive materials, the length-diameter ratio of the abrasive materials is 2-5, and the length of the abrasive materials is 5-10 micrometers; the abrasive used by the polishing solution II is diamond particles with the average particle size of 10 microns.
Comparative examples 1 and 2 the treatment conditions were the same as in examples 1 and 5, respectively, and the total duration of the polishing treatment was the same (20 min for comparative example 1; 30min for comparative example 2); except that only 10 micron diamond particles were used as the abrasive.
The surface roughness Ra of the aluminum oxide ceramic curved surface workpiece before treatment is 129.6nm, and the result after polishing treatment is shown in the following table 1:
TABLE 1
Figure 358419DEST_PATH_IMAGE001
The content of each raw material component is the percentage of the total mass of the polishing solution.

Claims (8)

1. A combined polishing solution is characterized by comprising two groups of independent polishing solutions I and II, wherein each group of polishing solution comprises 1-25% of abrasive and 75-99% of base solution by mass percent, the abrasive used by the polishing solution I is alumina whisker, SiC whisker, ZnO whisker and carbon fiber, the length-diameter ratio of the abrasive is 2-10, and the length of the abrasive is 5-10 micrometers; the grinding material used by the polishing solution II is superhard material particles with the average particle size of 0.5-50 microns, the superhard material is diamond particles, CBN particles or SiC particles,
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. The 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.
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CN109021835A (en) * 2018-09-03 2018-12-18 合肥久新不锈钢厨具有限公司 A kind of high-hardness stainless steel grinding and polishing liquid
CN109233646A (en) * 2018-11-02 2019-01-18 长沙县新光特种陶瓷有限公司 A kind of buffing wax and preparation method thereof
CN111761417A (en) * 2019-11-21 2020-10-13 苏州邦仕威五金科技有限公司 Hardware polishing process
CN113275953B (en) * 2021-06-11 2022-04-19 上海径驰精密工具有限公司 Polishing process of hard alloy cutting tool

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JP2001035819A (en) * 1999-07-16 2001-02-09 Nippei Toyama Corp Polishing slurry and polishing method using the same
CN102408757B (en) * 2011-09-15 2014-03-05 中国科学院金属研究所 Solvent-based nano silicon oxide concentrated pulp and preparation method thereof
CN102717325B (en) * 2012-06-08 2014-06-11 浙江工业大学 Ultra-precise curved surface finishing method based on non-Newtonian fluid shear thickening effect

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