CN108587479B - Sapphire polishing solution - Google Patents
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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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Abstract
The sapphire polishing solution is prepared from at least N-methyl pyrrolidone, alcohol amine, alcohol ether, fatty alcohol-polyoxyethylene ether, methylene dinaphthalene sodium sulfonate, transition metal oxide and water.
Description
Technical Field
The invention relates to the field of sapphire surface treatment, in particular to a sapphire polishing solution.
Background
The sapphire has the characteristics of high hardness, high melting point, good light transmittance, excellent heat conductivity and electrical insulation, stable chemical property and the like. The sapphire surface treatment method can be used for infrared light-transmitting materials of precision instruments and meters, windows and reflectors of lasers in the aerospace industry, epitaxial wafers of semiconductor silicon, epitaxial substrate materials of semiconductor GaN and integrated chips of insulating substrates, and has high requirements on the surface quality of sapphire.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a sapphire polishing solution, and the preparation raw materials at least comprise N-methyl pyrrolidone, alcohol amine, alcohol ether, fatty alcohol-polyoxyethylene ether, methylene dinaphthalene sodium sulfonate, transition metal oxide and water.
In some embodiments, the alcohol amine is selected from at least one of triisopropanolamine, diethanolamine, N-dibenzylethanol, N-butyldiethanolamine, triethanolamine, N-dibutylethanolamine, N- (phenoxyisopropyl) ethanolamine, N-methyldiethanolamine, N-dimethylethanolamine, ethylhydroxyethylamine, diisopropanolamine, oleoylethanolamide, N-phenylethanolamine, mandelic acid-diethanolamine, olive oil-diethanolamine, sesame oil-diethanolamine, wheat germ-diethanolamine, N-ethyldiethanolamine, triethanolamine lauryl sulfate, diallylethanolamine, phenylacetic acid-amine, triethanolamine laurate.
In some embodiments, the alcohol ether is selected from the group consisting of diethylene glycol methyl ethyl ether, ethylene glycol mono octyl ether, dimer ethylene glycol mono methyl amyl ether, dipropylene glycol monomethyl ether, propylene glycol methyl ether, ethylene glycol dimethyl ether, ethylene glycol monoethyl ether, 4-methoxy-1-butanol, 3-ethoxypropanol, diethylene glycol monomethyl ether, ethylene glycol monobutyl ether, diethylene glycol ethyl ether, diethylene glycol dimethyl ether, dipropylene glycol dimethyl ether, ethylene glycol monohexyl ether, diethylene glycol diethyl ether, triethylene glycol dimethyl ether, triethylene glycol monoethyl ether, diethylene glycol monohexyl ether, diethylene glycol dibutyl ether, dipropylene glycol methyl ether, ethylene glycol phenyl ether, propylene glycol monoallyl ether, tetraethylene glycol dimethyl ether, dipropylene glycol methyl ether, tetraethylene glycol monobutyl ether, dipropylene glycol monoethyl ether, propylene glycol butyl ether, dipropylene glycol methyl ether, ethylene glycol butyl ether, propylene, At least one of propylene glycol diglycidyl ether.
In some embodiments, the fatty alcohol-polyoxyethylene ether is selected from at least one of AEO-9, AEO-7, and AEO-3.
In some embodiments, the metal in the transition metal oxide is a lanthanide.
In some embodiments, the lanthanide is selected from at least one of lanthanum, cerium, neodymium, europium, erbium, thulium, ytterbium.
In some embodiments, the transition metal oxide is a mixture of a first transition metal oxide having a particle size of 10 to 30nm and a second transition metal oxide having a particle size of 30 to 60 nm.
In some embodiments, the weight ratio of the first transition metal oxide to the second transition metal oxide is 7: 2.
in some embodiments, polyvinylpyrrolidone is also included.
In some embodiments, the polyvinylpyrrolidone has an average molecular weight of 10000-.
Drawings
FIG. 1 is a nuclear magnetic resonance hydrogen spectrum obtained by centrifuging the sample of example 2 and drying the supernatant;
FIG. 2 is a chromatogram flowsheet of a headspace-gas chromatogram of example 2.
Detailed Description
For the purposes of the following detailed description, it is to be understood that the invention may assume various alternative variations and step sequences, except where expressly specified to the contrary. Moreover, other than in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties to be obtained by the present invention. At the very least, and not as an attempt to limit the application of the doctrine of equivalents to the scope of the claims, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Notwithstanding that the numerical ranges and parameters setting forth the broad scope of the invention are approximations, the numerical values set forth in the specific examples are reported as precisely as possible. Any numerical value, however, inherently contains certain errors necessarily resulting from the standard deviation found in their respective testing measurements.
Moreover, it should be understood that any numerical range recited herein is intended to include all sub-ranges subsumed therein. For example, a range of "1 to 10" is intended to include all sub-ranges between (and including) the recited minimum value of 1 and the recited maximum value of 10, i.e., having a minimum value equal to or greater than 1 and a maximum value of equal to or less than 10.
The invention provides a sapphire polishing solution, which is prepared from at least N-methyl pyrrolidone, alcohol amine, alcohol ether, fatty alcohol-polyoxyethylene ether, methylene dinaphthalene sodium sulfonate, transition metal oxide and water.
In some preferred embodiments, the raw materials for preparing the composite material at least comprise 0.1 to 1 part of N-methyl pyrrolidone, 0.1 to 0.8 part of alcohol amine, 0.05 to 0.5 part of alcohol ether, 0.1 to 1 part of fatty alcohol-polyoxyethylene ether, 0.05 to 0.5 part of methylene dinaphthalene sodium sulfonate, 50 to 80 parts of transition metal oxide and 30 to 40 parts of water in parts by weight.
In some preferred embodiments, the raw materials for preparing the composite material at least comprise 0.3 to 0.4 part of N-methyl pyrrolidone, 0.2 to 0.3 part of alcohol amine, 0.1 to 0.2 part of alcohol ether, 0.2 to 0.3 part of fatty alcohol-polyoxyethylene ether, 0.1 to 0.2 part of sodium methylene dinaphthalenesulfonate, 62 to 64 parts of transition metal oxide and 35 to 36 parts of water in parts by weight.
The sapphire has stable chemical property, good high temperature resistance and wear resistance, hardness second to that of diamond, and good dielectric property and thermal property. If the mechanical polishing method is used, only the sapphire can be polished using diamond powder, but the polishing efficiency is low and scratches are easily left on the sapphire surface. Chemical polishing mainly utilizes a chemical reagent to corrode the surface of a material, removes protrusions on the surface of the material, and enables the surface of the material to be smooth and flat.
According to different crystal growth directions, the sapphire can be divided into A-direction sapphire, C-direction sapphire and R-direction sapphire, wherein the most dense atomic surface is selected in the A-direction sapphire crystal growth direction.
In some embodiments, the sapphire is an a-directional sapphire.
In some embodiments, the alcohol amine is selected from at least one of triisopropanolamine, diethanolamine, N-dibenzylethanol, N-butyldiethanolamine, triethanolamine, N-dibutylethanolamine, N- (phenoxyisopropyl) ethanolamine, N-methyldiethanolamine, N-dimethylethanolamine, ethylhydroxyethylamine, diisopropanolamine, oleoylethanolamide, N-phenylethanolamine, mandelic acid-diethanolamine, olive oil-diethanolamine, sesame oil-diethanolamine, wheat germ-diethanolamine, N-ethyldiethanolamine, triethanolamine lauryl sulfate, diallylethanolamine, phenylacetic acid-amine, triethanolamine laurate.
In some preferred embodiments, the alcohol amine has a substituent on the nitrogen.
In a preferred embodiment of the present invention, the alcohol amine is at least one selected from the group consisting of N, N-dibenzylethanol, N-butyldiglycolamine, N-dibutylethanolamine, N- (phenoxyisopropyl) ethanolamine, N-methyldiethanolamine, N-dimethylethanolamine, N-ethyldiethanolamine, and N-phenylethanolamine.
In some embodiments, the alcohol ether is selected from the group consisting of diethylene glycol methyl ethyl ether, ethylene glycol mono octyl ether, dimer ethylene glycol mono methyl amyl ether, dipropylene glycol monomethyl ether, propylene glycol methyl ether, ethylene glycol dimethyl ether, ethylene glycol monoethyl ether, 4-methoxy-1-butanol, 3-ethoxypropanol, diethylene glycol monomethyl ether, ethylene glycol monobutyl ether, diethylene glycol ethyl ether, diethylene glycol dimethyl ether, dipropylene glycol dimethyl ether, ethylene glycol monohexyl ether, diethylene glycol diethyl ether, triethylene glycol dimethyl ether, triethylene glycol monoethyl ether, diethylene glycol monohexyl ether, diethylene glycol dibutyl ether, dipropylene glycol methyl ether, ethylene glycol phenyl ether, propylene glycol monoallyl ether, tetraethylene glycol dimethyl ether, dipropylene glycol methyl ether, tetraethylene glycol monobutyl ether, dipropylene glycol monoethyl ether, propylene glycol butyl ether, dipropylene glycol methyl ether, ethylene glycol butyl ether, propylene, At least one of propylene glycol diglycidyl ether.
In some embodiments, the fatty alcohol-polyoxyethylene ether is selected from at least one of AEO-9, AEO-7, and AEO-3.
In some embodiments, the metal in the transition metal oxide is a lanthanide.
In some embodiments, the lanthanide is selected from at least one of lanthanum, cerium, neodymium, europium, erbium, thulium, ytterbium.
In some embodiments, the transition metal oxide is a mixture of a first transition metal oxide having a particle size of 10 to 30nm and a second transition metal oxide having a particle size of 30 to 60 nm.
In some embodiments, the weight ratio of the first transition metal oxide to the second transition metal oxide is 7: 2.
in some embodiments, polyvinylpyrrolidone is also included.
In some embodiments, the polyvinylpyrrolidone has an average molecular weight of 10000-.
The polyvinylpyrrolidone can be purchased directly, for example, from Shanghai Co., Ltd of New tapping Bilk materials.
The inventor finds that the first transition metal oxide and the second transition metal oxide are mixed according to a certain particle size and weight ratio, so that good grading can be formed, a good polishing effect is achieved on A-direction sapphire, and the material removal rate can be improved. The inventors speculate that the first transition metal oxide and the second transition metal oxide have appropriate particle sizes, do not agglomerate, not only improve stability, but also improve dispersibility of the polishing composition, and positively affect improvement of the material removal rate. A generates a better soft layer on the surface of the sapphire under the grading of the first transition metal oxide and the second transition metal oxide, and the material removal rate is also improved.
The preparation method of the sapphire polishing solution comprises the steps of dissolving polyvinylpyrrolidone and sodium methylene dinaphthalene sulfonate in water, and fully stirring until the polyvinylpyrrolidone and the sodium methylene dinaphthalene sulfonate are completely dissolved; adding fatty alcohol-polyoxyethylene ether, alcohol amine, alcohol ether and N-methylpyrrolidone, and fully stirring until the mixture is completely dissolved; adding transition metal oxide, and stirring to mix well.
The invention is further illustrated by the following specific examples.
Example 1
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-90, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide and 35 parts of water. The particle size of cerium oxide was 25nm and the particle size of lanthanum oxide was 45 nm.
Example 2
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-0, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide, 35 parts of water and 250.3 parts of polyvinylpyrrolidone K. The particle size of cerium oxide was 25nm and the particle size of lanthanum oxide was 45 nm. The average molecular weight of polyvinylpyrrolidone K25 was 32000.
FIG. 1 is a nuclear magnetic resonance hydrogen spectrum obtained by centrifuging the sample of example 2 and drying the supernatant;
FIG. 2 is a chromatogram flowsheet of a headspace-gas chromatogram of example 2.
Example 3
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-0, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide, 35 parts of water and 250.3 parts of polyvinylpyrrolidone K. The particle size of cerium oxide was 5nm and the particle size of lanthanum oxide was 45 nm. The average molecular weight of polyvinylpyrrolidone K25 was 32000.
Example 4
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-0, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide, 35 parts of water and 250.3 parts of polyvinylpyrrolidone K. The particle size of cerium oxide was 45nm and the particle size of lanthanum oxide was 45 nm. The average molecular weight of polyvinylpyrrolidone K25 was 32000.
Example 5
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-0, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide, 35 parts of water and 250.3 parts of polyvinylpyrrolidone K. The particle size of cerium oxide is 25nm and the particle size of lanthanum oxide is 25 nm. The average molecular weight of polyvinylpyrrolidone K25 was 32000.
Example 6
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-0, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide, 35 parts of water and 250.3 parts of polyvinylpyrrolidone K. The particle size of cerium oxide is 25nm and the particle size of lanthanum oxide is 80 nm. The average molecular weight of polyvinylpyrrolidone K25 was 32000.
Example 7
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-0, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide, 35 parts of water and 300.3 parts of polyvinylpyrrolidone K. The particle size of cerium oxide was 25nm and the particle size of lanthanum oxide was 45 nm. Polyvinylpyrrolidone K30 had an average molecular weight of 37900.
Example 8
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-0, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 49 parts of cerium oxide, 14 parts of lanthanum oxide, 35 parts of water and 170.3 parts of polyvinylpyrrolidone K. The particle size of cerium oxide was 25nm and the particle size of lanthanum oxide was 45 nm. The average molecular weight of polyvinylpyrrolidone K17 was 10100.
Example 9
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-90, 0.1 part of methylene dinaphthalenesulfonic acid sodium, 63 parts of cerium oxide, 35 parts of water and 250.3 parts of polyvinylpyrrolidone K. The particle size of the cerium oxide was 25 nm. The average molecular weight of polyvinylpyrrolidone K25 was 32000.
Example 10
The sapphire polishing solution comprises, by weight, 0.3 part of N-methyl pyrrolidone, 0.2 part of N-methyldiethanolamine, 0.2 part of diethylene glycol dimethyl ether, 90.3 parts of fatty alcohol-polyoxyethylene ether AEO-90, 0.1 part of sodium methylene dinaphthalenesulfonate, 63 parts of lanthanum oxide, 35 parts of water and 250.3 parts of polyvinylpyrrolidone K. The particle size of lanthanum oxide was 45 nm. The average molecular weight of polyvinylpyrrolidone K25 was 32000.
Evaluation of stability
The samples 1-10 were stored in a sealed condition at 45 ℃ for 7 days, and the presence or absence of delamination was observed once a day, and the time of occurrence was recorded, and if no delamination occurred, it was recorded as none.
Material removal rate MRR evaluation
And polishing the sapphire in the A direction by using a grinding and polishing machine at the rotating speed of 70rpm and the temperature of 25 ℃ for 30 min.
And Δ m is the mass change before and after sapphire polishing, ρ is the sapphire density, S is the circular area of the sapphire wafer, and t is the polishing time.
The test results are listed in the following table.
The use of any and all examples, or exemplary language (e.g., "such as") provided herein, is intended merely to better illuminate the invention and does not pose a limitation on the scope of the invention unless otherwise claimed. No language in the specification should be construed as indicating any non-claimed element as essential to the practice of the invention.
Preferred embodiments of this invention are described herein, including the best mode known to the inventors for carrying out the invention. Variations of those preferred embodiments may become apparent to those of ordinary skill in the art upon reading the foregoing description. The inventors expect skilled artisans to employ such variations as appropriate, and the inventors intend for the invention to be practiced otherwise than as specifically described herein. Accordingly, this invention includes all modifications and equivalents of the subject matter recited in the claims appended hereto as permitted by applicable law. Moreover, any combination of the above-described elements in all possible variations thereof is encompassed by the invention unless otherwise indicated herein or otherwise clearly contradicted by context.
Claims (3)
1. The sapphire polishing solution is characterized by comprising, by weight, at least 0.3-0.4 part of N-methyl pyrrolidone, 0.2-0.3 part of alcohol amine, 0.1-0.2 part of alcohol ether, 0.2-0.3 part of fatty alcohol-polyoxyethylene ether, 0.1-0.2 part of methylene dinaphthalene sodium sulfonate, 62-64 parts of transition metal oxide and 35-36 parts of water;
the transition metal oxide is cerium oxide with the particle size of 10-25nm and lanthanum oxide with the particle size of 45-60nm, and the weight ratio of the cerium oxide to the lanthanum oxide is 7: 2;
the alcohol amine is selected from at least one of N, N-dibenzyl ethanol, N-butyl diethanolamine, N-dibutyl ethanolamine, N- (phenoxy isopropyl) ethanolamine, N-methyl diethanolamine, N-dimethyl ethanolamine, N-ethyl diethanolamine and N-phenyl ethanolamine;
also comprises polyvinylpyrrolidone; the average molecular weight of the polyvinylpyrrolidone is 10000-.
2. The sapphire polishing solution according to claim 1, wherein the alcohol ether is selected from the group consisting of diethylene glycol methyl ethyl ether, ethylene glycol mono octyl ether, dimeric ethylene glycol monomethyl amyl ether, dipropylene glycol monomethyl ether, propylene glycol methyl ether, ethylene glycol dimethyl ether, ethylene glycol monoethyl ether, 4-methoxy-1-butanol, 3-ethoxypropanol, diethylene glycol monomethyl ether, ethylene glycol monobutyl ether, diethylene glycol ethyl ether, diethylene glycol dimethyl ether, dipropylene glycol dimethyl ether, ethylene glycol monohexyl ether, diethylene glycol diethyl ether, triethylene glycol dimethyl ether, triethylene glycol monoethyl ether, diethylene glycol monohexyl ether, diethylene glycol dibutyl ether, dipropylene glycol methyl ether, ethylene glycol phenyl ether, propylene glycol monoallyl ether, tetraethylene glycol dimethyl ether, dipropylene glycol methyl propyl ether, tetraethylene glycol monobutyl ether, dipropylene glycol monoethyl ether, and mixtures thereof, At least one of propylene glycol butyl ether and propylene glycol diglycidyl ether.
3. The sapphire polishing solution according to claim 1, wherein the fatty alcohol-polyoxyethylene ether is at least one selected from the group consisting of AEO-9, AEO-7, and AEO-3.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102343547A (en) * | 2011-10-20 | 2012-02-08 | 天津理工大学 | Thermochemistry mechanical polishing method of sapphire substrate material and polishing solution |
| CN103013345A (en) * | 2012-12-21 | 2013-04-03 | 清华大学 | Oily diamond grinding liquid and preparation method thereof |
| CN107629701A (en) * | 2017-11-02 | 2018-01-26 | 东旭科技集团有限公司 | Polishing fluid and preparation method thereof |
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| JP2017190363A (en) * | 2016-04-11 | 2017-10-19 | 花王株式会社 | Polishing liquid composition for sapphire plate |
| CN108034360A (en) * | 2017-12-19 | 2018-05-15 | 北京创昱科技有限公司 | A kind of CMP planarization liquid and its application in GaAs wafer polishings |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102343547A (en) * | 2011-10-20 | 2012-02-08 | 天津理工大学 | Thermochemistry mechanical polishing method of sapphire substrate material and polishing solution |
| CN103013345A (en) * | 2012-12-21 | 2013-04-03 | 清华大学 | Oily diamond grinding liquid and preparation method thereof |
| CN107629701A (en) * | 2017-11-02 | 2018-01-26 | 东旭科技集团有限公司 | Polishing fluid and preparation method thereof |
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