CN116589929A - Composite polishing solution and preparation method and application thereof - Google Patents

Abstract

The application provides a compound polishing solution and a preparation method and application thereof, wherein the compound polishing solution comprises 86-97% of nano silica sol, 1-5% of alumina powder, 1-5% of suspension auxiliary agent, 0.1-1% of viscosity regulator, 0.1-1% of dispersing agent and 1-2% of pH regulator by mass percent; the composite polishing solution prepared by mixing silica sol and alumina powder according to a specific proportion and combining other auxiliary agents has excellent polishing performance and good storage stability.

Description

A kind of composite polishing liquid and its preparation method and application

technical field

The invention relates to the technical field of polishing liquid, and more specifically, to a composite polishing liquid and its preparation method and application.

Background technique

As one of the hardest substances in nature, sapphire has high hardness, corrosion resistance and excellent optical properties and is widely used in precision instruments, high-end lenses and semiconductor materials and other related fields. With the rapid development of science and technology, there are higher and higher requirements for fine processing and surface quality of sapphire surface. At present, the mainstream sapphire fine polishing process adopts the polishing liquid with silica as abrasive and the polishing liquid with alumina as abrasive, but the removal rate of silica polishing liquid for sapphire is low, while the removal rate of alumina polishing liquid for sapphire is low. The surface effect is poor after removal. Therefore, with the development of the industry, pure silica and alumina polishing fluids are increasingly unable to meet the industry's requirements for high removal rate and low surface roughness of sapphire. At present, many enterprises in the industry use multiple processes to polish sapphire, that is, first use alumina polishing liquid to grind sapphire to a certain thickness, and then use silicon oxide polishing liquid to make it reach a certain surface roughness. Or use composite polishing liquid, disclose a kind of preparation method of silicon-aluminum composite polishing liquid as Chinese patent application CN104046245A, this method is by adding aluminum oxide in silica sol, then adding viscosity regulator, pH regulator, polishing accelerator etc. However, in this composite polishing liquid, alumina is not considered as a nano-powder. Its surface activity is high, it is easy to agglomerate, and it is easy to cause defects such as scratches on the sapphire surface, and the polishing liquid is low in viscosity. It cannot be suspended stably, it is easy to stratify with water, silica sol, etc., and it cannot be stored stably, so that it affects its polishing effect.

Contents of the invention

Based on the above-mentioned technical problems in the prior art, the present invention provides a composite polishing liquid, which has an excellent polishing effect on sapphire and excellent stability.

In order to achieve the above object, the technical scheme of the present invention is as follows:

A kind of composite polishing fluid is characterized in that, by mass percentage, comprises following component:

In some embodiments, the particle diameter of the nano-silica sol is 50-150 nm, and the solid content is 20-40%.

In some embodiments, the crystal orientation of the alumina powder is α-direction, and the particle size is 100-300 nm.

In some embodiments, the suspension aid is at least one of acrylate copolymer, xanthan gum, gelatin, pectin, carboxymethylcellulose, carboxyethylcellulose, and hydroxypropylmethylcellulose .

In some embodiments, the viscosity modifier is at least one of ethylene glycol, propylene glycol, and glycerol.

In some embodiments, the dispersant is at least one of polyethylene glycol, sodium hexametaphosphate, sodium pyrophosphate, sodium tripolyphosphate, and sodium polyacrylate. Specifically, the polyethylene glycol includes but is not limited to polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and the like.

In some embodiments, the pH regulator is at least one of sodium hydroxide, potassium hydroxide, ethanolamine, triethanolamine, and ammonia water.

In some embodiments, the viscosity of the composite polishing liquid is 100-300 mPa·s.

The present invention also provides a method for preparing the composite polishing liquid of any of the above-mentioned embodiments, the method comprising the following steps:

S1, uniformly mixing the silica sol with a dispersant, a suspension aid, a viscosity regulator, and a pH regulator to obtain a first mixture;

S2, uniformly mixing the alumina powder and the first mixture to obtain a second mixture;

S3. Using an ultrasonic device to ultrasonically treat the second mixture for 10-20 minutes to obtain the composite polishing solution.

The present application also provides the application of the composite polishing liquid in any of the above embodiments in sapphire polishing.

Compared with the prior art, the beneficial effects of the present invention are as follows:

In the present invention, the composite polishing liquid with excellent polishing effect and good storage stability is obtained by compounding silica sol and alumina, and preparing in combination with specific suspension aids and other auxiliary agents. The composite polishing liquid provided by this application combines the characteristics of silica sol and alumina, combines the advantages and disadvantages of the two, and obtains a composite polishing liquid through a specific raw material ratio. The composite polishing liquid has a high removal rate and a high yield rate. , and the surface roughness of the treated sapphire is low, which can meet the high requirements of its application. In addition, through the composite polishing solution of the present application, the existing two polishing processes for sapphire can be shortened into one, which greatly improves production efficiency and reduces production cost.

Detailed ways

In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, the present invention can be implemented in many other ways different from those described here, and those skilled in the art can make similar improvements without departing from the connotation of the present invention, so the present invention is not limited by the specific implementations disclosed below.

Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention.

Example 1

The present embodiment provides a kind of preparation method of composite sapphire polishing liquid, and concrete steps are: get particle diameter and be 100nm, solid content is 953 parts of silica sols, add respectively 2 parts of polyethylene glycol 200, carboxyethyl fiber 10 parts of ethylene glycol, 5 parts of ethylene glycol, and 20 parts of sodium hydroxide are stirred evenly; then 10 parts of α-oriented alumina powder with a particle size of 100nm are added and stirred for 15 minutes, and the above-mentioned uniformly stirred slurry is put into an ultrasonic wave and stirred for 15 minutes , the ultrasonic frequency is 50Hz, and the composite polishing fluid with a viscosity of 200mPa·s is obtained.

Example 2

The present embodiment provides a kind of preparation method of composite sapphire polishing liquid, and concrete steps are: get particle diameter 100nm, solid content is 20-40% silica sol 924 parts, add respectively 2 parts of sodium hexametaphosphate, 20 parts of xanthan gum, 4 parts of propylene glycol and 20 parts of potassium hydroxide were stirred evenly; then 30 parts of α-oriented alumina powder with a particle size of 100nm were added and stirred for 15 minutes, and the above-mentioned uniformly stirred and dispersed slurry was put into an ultrasonic wave and stirred for 15 minutes, and the frequency of the ultrasonic wave was 50Hz. A composite polishing liquid with a viscosity of 150 mPa·s was obtained.

Example 3

The present embodiment provides a kind of preparation method of compound sapphire polishing liquid, and concrete steps are: get particle diameter 100nm, solid content is 925 parts of silica sols, add 2 parts of sodium tripolyphosphate, carboxymethyl cellulose 20 parts respectively 3 parts, 3 parts of glycerol, 20 parts of ethanolamine and stir evenly; then add 30 parts of α-oriented alumina powder with a particle size of 100nm and stir for 15 minutes, put the above-mentioned stirred and dispersed slurry into an ultrasonic wave and ultrasonically stir for 15 minutes, and the frequency of the ultrasonic wave is 50Hz to obtain a composite polishing fluid with a viscosity of 150mPa·s.

Example 4

The present embodiment provides a kind of preparation method of composite sapphire polishing liquid, and concrete steps are: take particle diameter 100nm, solid content be 903 parts of silica sol, add 2 parts of sodium polyacrylate, 20 parts of pectin, ethylene glycol respectively 5 parts of alcohol and 20 parts of triethanolamine were stirred evenly, and 50 parts of α-oriented alumina powder with a particle size of 100 nm were added and stirred for 15 minutes, and the above-mentioned uniformly stirred and dispersed slurry was ultrasonically stirred for 15 minutes, and the ultrasonic frequency was 50 Hz to obtain the viscosity Composite polishing liquid of 100mPa·s.

Comparative example 1

The present embodiment provides a kind of preparation method of composite sapphire polishing liquid, and concrete steps are: get particle diameter 100nm, solid content is 970 parts of silica sol, add polyethylene glycol 40010 parts, potassium hydroxide 20 parts respectively, Stir for 15 minutes, put the above uniformly stirred and dispersed slurry into an ultrasonic wave and ultrasonically stir for 15 minutes, and the frequency of the ultrasonic wave is 50 Hz to obtain a composite polishing solution with a viscosity of 200 mPa·s.

Comparative example 2

The present embodiment provides a kind of preparation method of composite sapphire polishing liquid, and concrete steps are: get 903 parts of deionized water, add respectively 2 parts of polyethylene glycol 600, 20 parts of xanthan gum, 5 parts of ethylene glycol, potassium hydroxide Stir 20 parts evenly, add 50 parts of α-oriented alumina powder with a particle size of 100 and stir for 15 minutes, put the above-mentioned uniformly stirred and dispersed slurry into ultrasonic waves for 15 minutes, and ultrasonic frequency is 50 Hz to obtain Compound polishing fluid.

Comparative example 3

This embodiment is based on the Chinese patent whose document number is CN 104046245 A, and provides a method for preparing a composite sapphire polishing solution. The specific steps are: take 820 parts of silica sol with a solid content of 40% and a particle diameter of 100nm, and add viscosities respectively 8 parts of conditioner, 163 parts of deionized water, 7 parts of polishing acceleration aid, 2 parts of pH regulator, stirred for 15 minutes, and the silica polishing liquid with the viscosity of 2-5 centipoise prepared above and the alumina with a particle size of 100 The polishing liquid is compounded according to the weight ratio of 18:1 to obtain the silicon-aluminum composite polishing liquid.

Comparative example 4

The present embodiment provides a kind of preparation method of composite sapphire polishing liquid, and concrete steps are: get particle diameter and be 100nm, solid content is 953 parts of silica sols, add respectively 2 parts of polyethylene glycol 200, carboxyethyl fiber 5 parts of ethylene glycol, 10 parts of ethylene glycol, and 20 parts of sodium hydroxide were stirred evenly; then 10 parts of α-oriented alumina powder with a particle size of 100 nm were added and stirred for 15 minutes, and the above-mentioned uniformly stirred slurry was put into an ultrasonic wave and stirred for 15 minutes , the ultrasonic frequency is 50Hz, and the composite polishing fluid with a viscosity of 200mPa·s is obtained.

Comparative example 5

The present embodiment provides a kind of preparation method of composite sapphire polishing liquid, and concrete steps are: get particle diameter and be 100nm, solid content is 953 parts of silica sols, add respectively 2 parts of polyethylene glycol 200, carboxyethyl fiber 70 parts of ethylene glycol, 5 parts of ethylene glycol, and 20 parts of sodium hydroxide are stirred evenly; then 10 parts of α-oriented alumina powder with a particle size of 100 nm are added and stirred for 15 minutes, and the above-mentioned uniformly stirred slurry is put into an ultrasonic wave and stirred for 15 minutes , the ultrasonic frequency is 50Hz, and the composite polishing fluid with a viscosity of 200mPa·s is obtained.

The polishing liquid that embodiment 1-4 and comparative example 1-3 obtain and pure water are mixed according to volume ratio 1:1, then process 4 inches C to sapphire sheet on 16B polisher (CJ company), use suba 600 polishing pad , the pressure is 5psi, the rotation speed of the lower plate is 55rpm, the flow rate of the polishing liquid is 10L/min, and the polishing time is 150min. The polishing data are shown in Table 1.

Table 1

Removal amount um Yield Surface roughness nm Example 1 20.5 94.08% 0.8 Example 2 24.8 93.95% 0.7 Example 3 25.1 93.81% 0.8 Example 4 28.9 95.02% 1.0 Comparative example 1 15.3 96.06% 0.6 Comparative example 2 26.3 93.13% 1.5 Comparative example 3 19.8 94.38% 1.2 Comparative example 4 20.3 93.91% 0.8 Comparative example 5 19.5 92.08% 1.3

Can know by the data of embodiment 1-4 and comparative example 1-2, pure silicon oxide polishing fluid removal rate is low, and surface roughness is low, and composite polishing fluid along with the increase of aluminum oxide powder addition, its removal rate has Obviously improved, although the roughness increases slightly, but the roughness of pure aluminum oxide polishing solution is significantly reduced, and the sapphire obtained by the compound polishing solution of the present application can meet the requirements of its practical application. Therefore, the composite polishing fluid can better meet the current requirements of high cutting and low surface roughness.

After the polishing liquid obtained in Examples 1-4 and Comparative Example 3 was left to stand at normal temperature and pressure for 30 days, the state of the polishing liquid was observed, and the data obtained were as shown in Table 2 below:

Table 2

From the comparative data of Examples 1-4 and Comparative Example 3, it can be known that the composite polishing liquid obtained by the present invention overcomes the characteristics that aluminum oxide is easily agglomerated as a nanopowder, so that the polishing liquid will not cause scratches during use. Injuries and other defects, and the polishing liquid can still be dispersed evenly and stored stably at low viscosity.

The polishing solution that was stored at room temperature and pressure for 30 days was used to process C-oriented sapphire in the above-mentioned manner, and the polishing data are shown in Table 3 below.

table 3

The technical features of the above-mentioned embodiments can be combined arbitrarily. To make the description concise, all possible combinations of the technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, should be considered as within the scope of this specification.

The above-mentioned embodiments only express several implementation modes of the present invention, and the descriptions thereof are relatively specific and detailed, but should not be construed as limiting the patent scope of the invention. It should be noted that, for those skilled in the art, several modifications and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the patent for the present invention should be based on the appended claims.

Claims (9)

1. a composite polishing liquid, is characterized in that, by mass percentage, comprises following component: 2. The composite polishing liquid according to claim 1, characterized in that, the particle size of the nano-silica sol is 50-150 nm, and the solid content is 20-40%. 3. The composite polishing liquid according to claim 1, characterized in that, the crystal orientation of the alumina powder is α-direction, and the particle size is 100-300 nm. 4. composite polishing fluid according to claim 1, is characterized in that, described suspending aid is acrylate copolymer, xanthan gum, gelatin, pectin, carboxymethyl cellulose, carboxyethyl cellulose, hydroxyl At least one of propyl methylcellulose. 5. The composite polishing liquid according to claim 1, characterized in that, the viscosity regulator is at least one of ethylene glycol, propylene glycol, and glycerol. 6. The composite polishing liquid according to claim 1, wherein the dispersant is at least one of polyethylene glycol, sodium hexametaphosphate, sodium pyrophosphate, sodium tripolyphosphate, and sodium polyacrylate. 7. The composite polishing fluid according to claim 1, wherein the pH regulator is at least one of sodium hydroxide, potassium hydroxide, ethanolamine, triethanolamine, and ammonia. 8. The preparation method of the composite polishing fluid described in any one of claims 1-7, is characterized in that, comprises the following steps: S1, uniformly mixing the silica sol with a dispersant, a suspension aid, a viscosity regulator, and a pH regulator to obtain a first mixture; S2. Mix the alumina powder and the first mixture uniformly to obtain a second mixture. S3. Use an ultrasonic device to ultrasonically treat the second mixture for 10-20 minutes to obtain the composite polishing solution. 9. the application of the composite polishing liquid described in any one of claims 1-7 on sapphire polishing.