CN111662642A - Sapphire polishing composition and preparation method thereof - Google Patents
Sapphire polishing composition and preparation method thereof Download PDFInfo
- Publication number
- CN111662642A CN111662642A CN202010666208.2A CN202010666208A CN111662642A CN 111662642 A CN111662642 A CN 111662642A CN 202010666208 A CN202010666208 A CN 202010666208A CN 111662642 A CN111662642 A CN 111662642A
- Authority
- CN
- China
- Prior art keywords
- polishing composition
- alkoxide
- sodium
- sapphire
- microcapsules
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention provides a sapphire polishing composition and a preparation method thereof. The composition takes silicon dioxide hydrosol as a main polishing component, and is added with alkoxide-ethyl cellulose microcapsules as an auxiliary agent. In addition, alkoxide-ethyl cellulose microcapsules are added into the polishing composition as an auxiliary agent, so that the corrosion rate of the sapphire can be increased, the polishing time can be shortened, and the polishing composition has remarkable advantages compared with the prior art.
Description
Technical Field
The invention relates to a polishing composition, in particular to a sapphire polishing composition and a preparation method thereof.
Background
The sapphire is corundum group mineral and the chemical component is Al2O3Transparent to translucent, glass luster, blue when containing trace elements of titanium or iron, belongs to a trigonal system, has the Mohs hardness of 9, is second to diamond, has large brittleness, is difficult to machine and has low efficiency. Sapphire, the hardest oxide crystal, is used in a variety of fields requiring special characteristics due to its unique optical and physical properties. Sapphire can maintain its high strength, excellent thermal properties and transmittance, excellent electrical and dielectric properties, and chemical resistance at high temperatures.
As important microelectronic and optoelectronic materials, sapphire is widely used in the blue (white) light LED illumination industry, in addition to the advanced technological fields of infrared devices, missiles, submarines, satellite space technology, detection, high-power intense laser, and the like, and sapphire single crystals are used as substrate materials in other technical fields with wider range toward higher end and higher precision along with the technological progress. The polishing solution for sapphire precision machining in the current market mainly takes silicon dioxide as a basic abrasive, and is combined with components such as a complexing agent, a surfactant, a dispersing agent and the like to realize high removal rate and planarization of sapphire, however, the mohs hardness of silicon dioxide abrasive particles is low, the mechanical action between the silicon dioxide abrasive particles and the sapphire is small, and the removal efficiency of the sapphire is low. Chinese published patents CN104046245B and CN102311706B propose adding alumina micro powder and diamond micro powder with higher hardness to silica hydrosol respectively to achieve ultra-high removal rate of sapphire, however, the high hardness abrasive particles and the sapphire wafer are prone to scratch on the surface of the sapphire wafer due to local high mechanical action therebetween, and the high isoelectric point of alumina in the aqueous solution is not favorable for stable dispersion in the alkaline silica hydrosol. Therefore, there is still a need to improve the composition of the polishing solution from the chemical formulation point of view to overcome the various drawbacks of the above-mentioned techniques under strong mechanical action.
Disclosure of Invention
In order to solve the technical problems, the invention provides a sapphire polishing composition and a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the sapphire polishing composition takes silicon dioxide hydrosol as a main polishing component and is added with alkoxide-ethyl cellulose microcapsules as an auxiliary agent. In the sapphire polishing process, the microcapsules are pressed to break to release alkoxide, after the alkoxide is contacted with water, on one hand, hydroxide radicals are released to quickly improve the alkalinity of the polishing solution, strengthen the chemical action of the sapphire surface and improve the corrosion rate of sapphire, on the other hand, a large amount of heat is released to improve the polishing working temperature, further promote the chemical reaction rate between the polishing composition and the sapphire and shorten the polishing time.
The invention does not limit any other auxiliary components added in the polishing composition, and the technicians can optionally select one or more of complexing agent, bacteriostatic agent, active agent, dispersing agent, wetting agent and rate accelerator to be added into the composition according to the requirements of further improving the sapphire polishing rate and surface quality.
The metal ions in the solution are complexed under the action of the complexing agent, so that the removal rate of the sapphire is increased, and the surface of the sapphire wafer is prevented from being contaminated by the metal ions; the bacteriostatic agent is used for inhibiting the formation and growth of microorganisms in the composition and prolonging the shelf life of the polishing composition; the active agent is used for reducing the surface tension of the composition and the contact angle between the composition and the sapphire, and the spreading performance of the composition on the surface of a sapphire wafer is improved; the dispersing agent is used as a surfactant, can prevent the silica hydrosol from settling and condensing, and is favorable for promoting the uniform dispersion of all material components to form stable suspension.
Further, the silica hydrosol has a particle size of 50 to 120nm and a concentration of 10 to 50 wt%, preferably 30 to 50 wt%.
Further, the alkoxide is at least one of sodium ethoxide, potassium ethoxide, sodium methoxide and potassium methoxide.
Further, the composition is prepared from the following components in parts by weight:
preferably, the mass ratio of the alkoxide to the ethylcellulose in the alkoxide-ethylcellulose microcapsules is 0.1 to 1; the microcapsule particle size is preferably 1 to 10 μm.
Further, the complexing agent is at least one of glycine, citric acid, tartaric acid, ethylene diamine tetraacetic acid, ethylene diamine tetra methylene phosphonic acid, nitrilotriacetic acid and salts thereof.
Further, the bacteriostatic agent is at least one of 1, 2-benzisothiazolin-3-one (BIT), 2-n-octyl-4-isothiazolin-3-One (OIT), 2-methyl-4-isothiazolin-3-one (MIT) and 5-chloro-2-methyl-4-isothiazolin-3-one (CMIT).
Further, the active agent is at least one of dodecyl trimethyl ammonium chloride, fatty alcohol polyoxyethylene ether (AEO), nonylphenol polyoxyethylene ether, polyoxyethylene alkylamine, alkylol phthalein amine, fatty acid polyoxyethylene ether, fatty ammonium polyoxyethylene ether, polyoxyethylene lauryl ether, sodium methylene dinaphthalene sulfonate, Alkylphenol Polyoxyethylene Ether (APEO), sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
Further, the dispersant is at least one of polyacrylic acid, sodium polyacrylate, sodium pyrophosphate, sodium hexametaphosphate and polyethylene glycol, and the molecular weight of the polyethylene glycol is 400-2000-.
A method for preparing a sapphire polishing composition comprises the steps of mixing a silicon dioxide hydrosol and alkoxide-ethylcellulose microcapsules in deionized water; the alkoxide-ethylcellulose microcapsules are preferably fully dispersed and then mixed with silica hydrosol; the dispersing means includes, but is not limited to, any one or more of ultrasonic dispersion, stirring, and rotational dispersion.
The alkoxide-ethylcellulose microcapsules are prepared by uniformly dispersing alkoxide and ethylcellulose in an organic solvent and then carrying out spray drying; the uniform dispersion mode can be any one or more of ultrasonic dispersion, stirring and rotating dispersion, and the invention does not limit the dispersion method on the basis of meeting the dispersion requirement.
Preferably, the organic solvent is at least one of benzene, toluene, xylene, pentane, hexane, octane, anhydrous methanol, anhydrous ethanol, isopropanol, diethyl ether, methyl acetate, ethyl acetate and propyl acetate.
Further, in the process of mixing the silicon dioxide hydrosol and the alkoxide-ethylcellulose microcapsules, a complexing agent, a bacteriostatic agent, an activating agent and a dispersing agent are added to form a composite dispersion liquid;
and adjusting the pH value of the composite dispersion liquid to 9-13, preferably 9-11, discharging and storing. It is to be specifically noted that the pH adjusting agent used in the pH adjustment of the present invention does not react with other components of the polishing composition or cause material failure, and preferably an alkaline substance is used as the pH adjusting agent, and more preferably at least one of sodium hydroxide, potassium hydroxide, ethylenediamine, hydroxyethylethylenediamine, ethanolamine, tetraethylammonium hydroxide, and tetramethylammonium hydroxide, based on the above-mentioned material formulation. The concentration of the pH adjusting agent is preferably in the range of 1 to 10 wt%.
In addition, alkoxide-ethyl cellulose microcapsules are added into the polishing composition as an auxiliary agent, so that the corrosion rate of the sapphire can be increased, the polishing time can be shortened, and the polishing composition has remarkable advantages compared with the prior art.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be illustrative of the invention and are not to be construed as limiting the scope of the invention.
In the following examples, the instruments and parameters used in the polishing test of the sapphire substrate material are shown in table 1:
TABLE 1 instruments and parameters used for polishing tests
Unless otherwise specified, the raw materials and reagents used in the examples of the present invention and comparative examples were obtained commercially.
[ example 1 ]
(1) Preparation of Potassium ethoxide-Ethyl cellulose microcapsules
Dissolving 500g of ethyl cellulose in 2kg of toluene solvent, continuously adding 50g of potassium ethoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotation speed of a centrifugal atomizer to be 18000rpm, and preparing the potassium ethoxide-ethyl cellulose microcapsule with the particle size of 1-10 mu m.
(2) Dispensing polishing composition
Firstly, adding 5g of potassium ethoxide-ethyl cellulose microcapsules into 500g of deionized water, and performing ultrasonic dispersion for 30min to prepare a suspension; the suspension was added to 1000g of a 10 wt% silica hydrosol (average particle size 80nm) with stirring;
adding 2.5g of glycine, 0.5g of sodium dodecyl benzene sulfonate, 0.5g of 1, 2-benzisothiazolin-3-one and 0.5g of polyacrylic acid into 100mL of deionized water for dissolving, completely adding the mixture into the suspension, uniformly stirring, and continuously adding the deionized water until the total amount of the solution is 5 kg; then, 1 wt% KOH was used as a pH adjuster to adjust the pH to 9.
[ example 2 ]
(1) Preparation of sodium ethoxide-ethyl cellulose microcapsules
Dissolving 100g of ethyl cellulose in 2kg of toluene solvent, continuously adding 100g of sodium ethoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotating speed of a centrifugal atomizer to be 18000rpm, and obtaining the sodium ethoxide-ethyl cellulose microcapsule with the particle size range of 1-10 mu m.
(2) Dispensing polishing composition
Firstly, adding 25g of sodium ethoxide-ethyl cellulose microcapsules into 500g of deionized water, and performing ultrasonic dispersion for 30min to prepare a suspension; the suspension was added to 1500g of a 25 wt% silica hydrosol (average particle size 80nm) with stirring;
adding 5g of citric acid, 2.5g of dodecyl trimethyl ammonium chloride, 2.5g of 2-n-octyl-4-isothiazoline-3-ketone and 2.5g of sodium polyacrylate into 100mL of deionized water for dissolving, completely adding the mixture into the suspension, uniformly stirring, and continuously adding the deionized water until the total amount of the solution is 5 kg; then, pH was adjusted to 10 with 5 wt% NaOH as a pH adjuster.
[ example 3 ]
(1) Preparation of Potassium methoxide-Ethyl cellulose microcapsules
Dissolving 200g of ethyl cellulose in 2kg of toluene solvent, continuously adding 100g of potassium methoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotating speed of a centrifugal atomizer to be 18000rpm, and obtaining the potassium methoxide-ethyl cellulose microcapsule with the particle size range of 1-10 mu m.
(2) Dispensing polishing composition
Firstly, 100g of potassium methoxide-ethyl cellulose microcapsules are added into 500g of deionized water, and the mixture is ultrasonically dispersed for 30min to prepare suspension; this suspension was added to 2500g of a 50 wt% silica hydrosol (average particle diameter 100nm) with stirring;
adding 25g of sodium citrate, 25g of fatty alcohol-polyoxyethylene ether, 25g of 2-methyl-4-isothiazoline-3-ketone and 25g of sodium pyrophosphate into 500mL of deionized water for dissolving, completely adding the mixture into the suspension, uniformly stirring, and continuously adding the deionized water until the total amount of the solution is 5 kg; then, 10 wt% of ethylenediamine was used as a pH adjuster to adjust the pH to 11.
[ example 4 ]
(1) Preparation of sodium methoxide-ethylcellulose microcapsules
Dissolving 500g of ethyl cellulose in 2kg of toluene solvent, continuously adding 100g of sodium methoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotation speed of a centrifugal atomizer to be 18000rpm, and obtaining the sodium methoxide-ethyl cellulose microcapsule with the particle size range of 1-10 mu m.
(2) Dispensing polishing composition
Firstly, adding 250g of sodium methoxide-ethyl cellulose microcapsules into 500g of deionized water, and ultrasonically dispersing for 30min to prepare suspension; this suspension was added to 3000g of a 40 wt% silica hydrosol (average particle size 120nm) with stirring;
adding 50g of disodium ethylene diamine tetraacetate, 50g of nonylphenol polyoxyethylene ether, 250g of 5-chloro-2-methyl-4-isothiazolin-3-one and 50g of sodium hexametaphosphate into 500mL of deionized water for dissolving, completely adding the mixture into the suspension, uniformly stirring, and continuously adding the deionized water until the total amount of the solution is 5 kg; then, 10 wt% of hydroxyethyl ethylenediamine is used as a pH regulator to regulate the pH to 11.
[ example 5 ]
(1) Preparation of sodium ethoxide-ethyl cellulose microcapsules
Dissolving 700g of ethyl cellulose in 2kg of toluene solvent, continuously adding 100g of sodium ethoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotating speed of a centrifugal atomizer to be 18000rpm, and obtaining the sodium ethoxide-ethyl cellulose microcapsule with the particle size range of 1-10 mu m.
(2) Dispensing polishing composition
Firstly, adding 75g of sodium ethoxide-ethyl cellulose microcapsules into 500g of deionized water, and performing ultrasonic dispersion for 30min to prepare a suspension; the suspension was added to 2000g of a 40 wt% silica hydrosol (average particle size 100nm) with stirring;
adding 26.25g of tartaric acid, 25.25g of polyoxyethylene alkylamine, 25.25g of 1, 2-benzisothiazolin-3-one and 25.25g of polyethylene glycol 400 into 500mL of deionized water for dissolving, completely adding the mixture into the suspension, uniformly stirring, and continuously adding the deionized water until the total amount of the solution is 5 kg; then, 10 wt% of ethanolamine is used as a pH regulator to regulate the pH to 10.5.
[ example 6 ]
(1) Preparation of Potassium methoxide-Ethyl cellulose microcapsules
Dissolving 200g of ethyl cellulose in 2kg of toluene solvent, continuously adding 100g of potassium methoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotating speed of a centrifugal atomizer to be 18000rpm, and obtaining 300g of potassium methoxide-ethyl cellulose microcapsules with the particle size range of 1-10 mu m
(2) Dispensing polishing composition
Firstly, 62.5g of potassium methoxide-ethyl cellulose microcapsules are added into 500g of deionized water, and ultrasonic dispersion is carried out for 30min to prepare suspension; this suspension was added to 2500g of a 40 wt% silica hydrosol (average particle diameter 100nm) with stirring;
adding 12.5g of ethylenediamine methylene phosphonic acid sodium, 13.75g of alkylol phthalide amine, 13.75g of 1, 2-benzisothiazolin-3-one and 13.75g of polyethylene glycol 600 into 500mL of deionized water for dissolving, completely adding the mixture into the suspension, uniformly stirring, and continuously adding the deionized water until the total amount of the solution is 5 kg; then, the pH was adjusted to 10.5 with 10 wt% tetraethylammonium hydroxide as a pH adjuster.
[ example 7 ]
(1) Preparation of sodium ethoxide-ethyl cellulose microcapsules
Dissolving 200g of ethyl cellulose in 2kg of toluene solvent, continuously adding 100g of sodium ethoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotating speed of a centrifugal atomizer to be 18000rpm, and obtaining 300g of sodium ethoxide-ethyl cellulose microcapsules with the particle size range of 1-10 mu m
(2) Dispensing polishing composition
Firstly, 50g of sodium ethoxide-ethyl cellulose microcapsules are added into 500g of deionized water, and ultrasonic dispersion is carried out for 30min to prepare suspension; this suspension was added to 2500g of a 40 wt% silica hydrosol (average particle diameter 100nm) with stirring;
adding 10g of sodium aminotriacetate, 5g of fatty acid polyoxyethylene ether, 0.7g of 1, 2-benzisothiazolin-3-one and 5g of polyethylene glycol 1000 into 500mL of deionized water for dissolving, completely adding the mixture into the suspension, uniformly stirring, and continuously adding the deionized water until the total amount of the solution is 5 kg; then, 10 wt% of tetramethylammonium hydroxide was used as a pH adjuster to adjust the pH to 10.5.
[ example 8 ]
(1) Preparation of sodium ethoxide-ethyl cellulose microcapsules
Dissolving 200g of ethyl cellulose in 2kg of toluene solvent, continuously adding 100g of sodium ethoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotating speed of a centrifugal atomizer to be 18000rpm, and obtaining 300g of sodium ethoxide-ethyl cellulose microcapsules with the particle size range of 1-10 mu m
(2) Dispensing polishing composition
Firstly, 100g of sodium ethoxide-ethyl cellulose microcapsules are added into 500g of deionized water, and the mixture is subjected to ultrasonic dispersion for 30min to prepare a suspension; this suspension was added to 2500g of a 40 wt% silica hydrosol (average particle diameter 100nm) with stirring; stirring evenly, continuously adding deionized water until the total amount of the solution is 5kg, and adjusting the pH to 10.5 by taking 10 wt% of KOH as a pH regulator.
[ example 9 ]
(1) Preparation of sodium ethoxide-ethyl cellulose microcapsules
Dissolving 200g of ethyl cellulose in 2L of toluene solvent, continuously adding 100g of sodium ethoxide, performing ultrasonic dispersion for 30min, introducing the mixed solution into a feeding pipeline of a spray dryer by using a pump, setting the inlet temperature to be 150 ℃, the outlet temperature to be 80 ℃ and the rotating speed of a centrifugal atomizer to be 18000rpm, and obtaining 300g of sodium ethoxide-ethyl cellulose microcapsules with the particle size range of 1-10 mu m.
(2) Dispensing polishing composition
Firstly, 100g of sodium ethoxide-ethyl cellulose microcapsules are added into 500g of deionized water, and the mixture is subjected to ultrasonic dispersion for 30min to prepare a suspension; this suspension was added to 2500g of a 40 wt% silica hydrosol (average particle diameter 100nm) with stirring;
adding 25g of sodium citrate into 500mL of deionized water to dissolve, adding all the sodium citrate into the suspension, stirring uniformly, continuously adding deionized water until the total amount of the solution is 5kg, and adjusting the pH to 11 by taking 10 wt% of ethylenediamine as a pH regulator.
Comparative example 1
Configuring a microcapsule-free polishing composition:
10g of sodium aminotriacetate, 5g of fatty acid polyoxyethylene ether, 0.7g of 1, 2-benzisothiazolin-3-one and 5g of polyethylene glycol 1000 are added into 500mL of deionized water to be dissolved, then all the materials are added into 2500g of 40 wt% silicon dioxide hydrosol (the average particle size is 100nm), the mixture is uniformly stirred, the deionized water is continuously added until the total amount of the solution is 5kg, and 10 wt% tetramethyl ammonium hydroxide is used as a pH regulator to regulate the pH value to 10.5.
Comparative example 2
The microcapsules were mixed with the silica hydrosol without dispersion to prepare the polishing composition:
the sodium ethoxide-ethylcellulose microcapsules prepared in example 2 were directly added to the silica hydrosol, and the amounts of the other materials and the preparation process were the same as those in example 2, to prepare a polishing composition.
Comparative example 3
Alkoxide was added directly to the silica hydrosol to prepare a polishing composition:
adding 25g of sodium citrate, 25g of fatty alcohol-polyoxyethylene ether, 25g of 2-methyl-4-isothiazoline-3-ketone, 25g of sodium pyrophosphate and 100g of potassium methoxide into 500mL of deionized water for dissolving, then completely adding the dissolved solution into 2500g of 40 wt% silicon dioxide hydrosol (the average particle size is 100nm), uniformly stirring, continuously adding deionized water until the total amount of the solution is 5kg, and adjusting the pH to 11 by taking 10 wt% phosphoric acid as a pH regulator.
Polishing the same type of sapphire substrate material by using the polishing instruments and parameters shown in Table 1; the polishing rate was evaluated by measuring the difference in mass between before and after the sapphire polishing with a balance, and the surface roughness was evaluated by measuring the arithmetic mean deviation Ra of the profile of the surface of the sapphire substrate material with an AFM atomic force microscope. The results of the polishing tests of the examples and comparative examples are shown in table 2:
TABLE 2 results of polishing test
| Polishing composition | Removal Rate (. mu.m/h) | Surface roughness Ra (nm) |
| Example 1 | 3.0 | 0.31 |
| Example 2 | 3.3 | 0.36 |
| Example 3 | 3.9 | 0.39 |
| Example 4 | 4.0 | 0.35 |
| Example 5 | 3.8 | 0.35 |
| Example 6 | 3.7 | 0.37 |
| Example 7 | 3.9 | 0.32 |
| Example 8 | 3.1 | 0.31 |
| Example 9 | 3.9 | 0.41 |
| Comparative example 1 | 1.9 | 0.42 |
| Comparative example 2 | 2.8 | 0.51 |
| Comparative example 3 | 2.0 | 0.45 |
It is clear from comparison of examples 1 to 9 with comparative example 1 that the addition of alkoxide-ethylcellulose microcapsules effectively increases the removal rate of sapphire. As can be seen from comparison between example 2 and comparative example 2, the addition of alkoxide-ethylcellulose microcapsules directly to the silica hydrosol without dispersion increases the surface roughness of the polished sapphire wafer, which is presumed to be due to local excessive corrosion of the surface of the sapphire wafer caused by uneven distribution of the alkoxide-ethylcellulose microcapsules in the silica sol. Comparing examples 1-9 with comparative example 3, it can be seen that the addition of alkoxide directly to the silica hydrosol did not provide the effect of increasing the polishing rate of sapphire wafers.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and additions can be made without departing from the method of the present invention, and these modifications and additions should also be regarded as the protection scope of the present invention.
Claims (10)
1. The sapphire polishing composition is characterized in that silicon dioxide hydrosol is used as a main polishing component, and alkoxide-ethyl cellulose microcapsules are added as an auxiliary agent.
2. The sapphire polishing composition of claim 1, wherein the silica hydrosol has a particle size of 50-120nm and a concentration of 10-50 wt.%, preferably 30-50 wt.%.
3. The sapphire polishing composition of claim 2, wherein the alkoxide is at least one of sodium ethoxide, potassium ethoxide, sodium methoxide, and potassium methoxide.
4. The sapphire polishing composition of any one of claims 1-3, wherein the composition is prepared from the following components in parts by weight:
preferably, the mass ratio of the alkoxide to the ethylcellulose in the alkoxide-ethylcellulose microcapsules is 0.1 to 1.
5. The sapphire polishing composition of claim 3 or 4, wherein the complexing agent is at least one of glycine, citric acid, tartaric acid, ethylenediaminetetraacetic acid, ethylenediaminetetramethylenephosphonic acid, nitrilotriacetic acid, and salts thereof.
6. The sapphire polishing composition of any one of claims 3-5, wherein the bacteriostatic agent is at least one of 1, 2-benzisothiazolin-3-one, 2-n-octyl-4-isothiazolin-3-one, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one.
7. The sapphire polishing composition of any one of claims 3-6, wherein the active agent is at least one of dodecyltrimethylammonium chloride, fatty alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, polyoxyethylene alkylamine, alkylolphthalein amine, fatty acid polyoxyethylene ether, fatty ammonium polyoxyethylene ether, polyoxyethylene lauryl ether, sodium methylene dinaphthalene sulfonate, alkylphenol polyoxyethylene ether, sodium dodecylbenzenesulfonate, sodium lauryl sulfate.
8. The sapphire polishing composition of any one of claims 3-7, wherein the dispersant is at least one of polyacrylic acid, sodium polyacrylate, sodium pyrophosphate, sodium hexametaphosphate, and polyethylene glycol, and the molecular weight of the polyethylene glycol is 400-.
9. A method of preparing the sapphire polishing composition of any one of claims 1-8, comprising the steps of mixing a silica hydrosol with alkoxide-ethylcellulose microcapsules in deionized water; the alkoxide-ethylcellulose microcapsules are preferably fully dispersed and then mixed with silica hydrosol;
the alkoxide-ethylcellulose microcapsules are prepared by uniformly dispersing alkoxide and ethylcellulose in an organic solvent and then carrying out spray drying; preferably, the organic solvent is at least one of benzene, toluene, xylene, pentane, hexane, octane, anhydrous methanol, anhydrous ethanol, isopropanol, diethyl ether, methyl acetate, ethyl acetate and propyl acetate.
10. The preparation method according to claim 9, wherein a complexing agent, a bacteriostatic agent, an activator and a dispersing agent are further added in the process of mixing the silica hydrosol and the alkoxide-ethylcellulose microcapsules to form a composite dispersion liquid;
and adjusting the pH value of the composite dispersion liquid to 9-13, preferably 9-11, discharging and storing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010666208.2A CN111662642B (en) | 2020-07-13 | 2020-07-13 | Sapphire polishing composition and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010666208.2A CN111662642B (en) | 2020-07-13 | 2020-07-13 | Sapphire polishing composition and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111662642A true CN111662642A (en) | 2020-09-15 |
| CN111662642B CN111662642B (en) | 2021-07-23 |
Family
ID=72392175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010666208.2A Active CN111662642B (en) | 2020-07-13 | 2020-07-13 | Sapphire polishing composition and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111662642B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112680113A (en) * | 2020-12-29 | 2021-04-20 | 北京航天赛德科技发展有限公司 | Composition for sapphire double-sided polishing and preparation method and application thereof |
| CN113416493A (en) * | 2021-06-02 | 2021-09-21 | 万华化学集团电子材料有限公司 | Preparation method of silicon wafer polishing composition with stable storage, composition and use method thereof |
| CN113637413A (en) * | 2021-09-02 | 2021-11-12 | 万华化学集团电子材料有限公司 | Silicon polishing composition, preparation method and application thereof |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004071918A (en) * | 2002-08-08 | 2004-03-04 | Okamoto Machine Tool Works Ltd | Chemical mechanical polishing tool for substrate and its forming method |
| CN101758463A (en) * | 2010-02-25 | 2010-06-30 | 浙江工业大学 | Self-lubricating grinding tool and preparation method thereof |
| JP2011103410A (en) * | 2009-11-11 | 2011-05-26 | Kuraray Co Ltd | Slurry for chemical mechanical polishing |
| CN102115633A (en) * | 2009-12-30 | 2011-07-06 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid |
| CN102453436A (en) * | 2010-10-22 | 2012-05-16 | 安集微电子（上海）有限公司 | Polishing composition |
| CN104004206A (en) * | 2014-05-09 | 2014-08-27 | 河南科技大学 | Cellulose solvent, and preparation method and application thereof |
| CN104798181A (en) * | 2012-11-30 | 2015-07-22 | 霓达哈斯股份有限公司 | Polishing composition |
| CN105385357A (en) * | 2015-12-11 | 2016-03-09 | 蓝思科技（长沙）有限公司 | Polishing solution for A orientation sapphire polishing, and preparation method thereof |
| CN107987731A (en) * | 2017-12-19 | 2018-05-04 | 北京航天赛德科技发展有限公司 | A kind of polishing fluid for sapphire 3D polishings and preparation method thereof |
| KR20180068682A (en) * | 2016-12-14 | 2018-06-22 | 에프엔에스테크 주식회사 | Polishing pad and preparing method thereof |
| CN108485532A (en) * | 2018-04-23 | 2018-09-04 | 江苏金琥珀光学科技股份有限公司 | The sapphire polishing liquid and its polishing process of high surface smoothness |
| CN109666410A (en) * | 2019-02-02 | 2019-04-23 | 上海映智研磨材料有限公司 | Sapphire polishing liquid additive and its preparation method and application |
| CN110003798A (en) * | 2019-05-20 | 2019-07-12 | 广东惠尔特纳米科技有限公司 | A kind of polishing fluid and its preparation method and application |
| WO2019210125A1 (en) * | 2018-04-27 | 2019-10-31 | International Flavors & Fragrances Inc. | Stable polyurea microcapsule compositions |
-
2020
- 2020-07-13 CN CN202010666208.2A patent/CN111662642B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004071918A (en) * | 2002-08-08 | 2004-03-04 | Okamoto Machine Tool Works Ltd | Chemical mechanical polishing tool for substrate and its forming method |
| JP2011103410A (en) * | 2009-11-11 | 2011-05-26 | Kuraray Co Ltd | Slurry for chemical mechanical polishing |
| CN102115633A (en) * | 2009-12-30 | 2011-07-06 | 安集微电子（上海）有限公司 | Chemical mechanical polishing liquid |
| CN101758463A (en) * | 2010-02-25 | 2010-06-30 | 浙江工业大学 | Self-lubricating grinding tool and preparation method thereof |
| CN102453436A (en) * | 2010-10-22 | 2012-05-16 | 安集微电子（上海）有限公司 | Polishing composition |
| CN104798181A (en) * | 2012-11-30 | 2015-07-22 | 霓达哈斯股份有限公司 | Polishing composition |
| CN104004206A (en) * | 2014-05-09 | 2014-08-27 | 河南科技大学 | Cellulose solvent, and preparation method and application thereof |
| CN105385357A (en) * | 2015-12-11 | 2016-03-09 | 蓝思科技（长沙）有限公司 | Polishing solution for A orientation sapphire polishing, and preparation method thereof |
| KR20180068682A (en) * | 2016-12-14 | 2018-06-22 | 에프엔에스테크 주식회사 | Polishing pad and preparing method thereof |
| CN107987731A (en) * | 2017-12-19 | 2018-05-04 | 北京航天赛德科技发展有限公司 | A kind of polishing fluid for sapphire 3D polishings and preparation method thereof |
| CN108485532A (en) * | 2018-04-23 | 2018-09-04 | 江苏金琥珀光学科技股份有限公司 | The sapphire polishing liquid and its polishing process of high surface smoothness |
| WO2019210125A1 (en) * | 2018-04-27 | 2019-10-31 | International Flavors & Fragrances Inc. | Stable polyurea microcapsule compositions |
| CN109666410A (en) * | 2019-02-02 | 2019-04-23 | 上海映智研磨材料有限公司 | Sapphire polishing liquid additive and its preparation method and application |
| CN110003798A (en) * | 2019-05-20 | 2019-07-12 | 广东惠尔特纳米科技有限公司 | A kind of polishing fluid and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 焦利勇: "微胶囊技术在印刷油墨中的应用 ", 《包装工程》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112680113A (en) * | 2020-12-29 | 2021-04-20 | 北京航天赛德科技发展有限公司 | Composition for sapphire double-sided polishing and preparation method and application thereof |
| CN113416493A (en) * | 2021-06-02 | 2021-09-21 | 万华化学集团电子材料有限公司 | Preparation method of silicon wafer polishing composition with stable storage, composition and use method thereof |
| CN113637413A (en) * | 2021-09-02 | 2021-11-12 | 万华化学集团电子材料有限公司 | Silicon polishing composition, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111662642B (en) | 2021-07-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111662642B (en) | Sapphire polishing composition and preparation method thereof | |
| WO2019119816A1 (en) | Cmp polishing solution, preparation method therefor and application thereof | |
| CN103450812B (en) | Polishing solution for sapphire substrate | |
| US8114178B2 (en) | Polishing composition for semiconductor wafer and polishing method | |
| CN103571333B (en) | CMP (Chemical-Mechanical Polishing) polishing liquid with mixed grinding materials for alkaline sapphire substrate and preparation method thereof | |
| KR100628019B1 (en) | Edge polishing composition | |
| CN107189693B (en) | Polishing solution for chemical mechanical polishing of A-direction sapphire and preparation method thereof | |
| CN100556619C (en) | Method for controlling surface roughness of sapphire substrate material | |
| CN102127371B (en) | Preparation method and use method of polishing solution for silicon carbide | |
| CN105038607A (en) | Effective sapphire fine grinding method and fine grinding solution | |
| CN113549399B (en) | Chemical mechanical polishing composition suitable for rough polishing of silicon wafer and application thereof | |
| CN104745146A (en) | Nano-composite abrasive particle sol containing cerium-doped silicon dioxide, polishing agent and preparation method thereof | |
| US20080135520A1 (en) | Chemical composition for chemical mechanical planarization | |
| CN112521864A (en) | Chemical mechanical polishing solution for semiconductor silicon carbide chip | |
| CN107936848B (en) | Polishing solution for polishing silicon substrate and preparation method thereof | |
| CN101912855A (en) | Surface cleaning method after sapphire substrate material polishing | |
| JP2004203638A (en) | Peanut-like twin colloidal silica particle, and production method therefor | |
| CN104531067B (en) | A kind of hydridization abrasive material and preparation method and the purposes in Ultraprecise polished | |
| CN114456716B (en) | Aluminum oxide polishing solution for polishing sapphire and preparation method thereof | |
| CN102399496A (en) | Abrasive composition for rough polishing of wafers | |
| CN108300330A (en) | A kind of ceramic wafers surface polishing slurries and preparation method thereof | |
| CN111073518B (en) | Preparation method of silicon-aluminum composite polishing powder | |
| CN109943235B (en) | Water-based composite polishing solution for ceramic polishing and preparation method thereof | |
| CN109679506A (en) | A kind of SiC single crystal piece essence throwing water base polishing fluid and preparation method thereof | |
| JP2003055648A (en) | Polishing agent and method for polishing substrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20201022 Address after: No. 50, Beijing Middle Road, Yantai Economic and Technological Development Zone, Shandong Province Applicant after: Wanhua Chemical Group Electronic Materials Co., Ltd Address before: 264006 No. 17 Tianshan Road, Yantai economic and Technological Development Zone, Shandong Applicant before: Wanhua Chemical Group Co.,Ltd. |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |