CN107541145B - Green environment-friendly polishing silica sol and preparation method thereof - Google Patents
Green environment-friendly polishing silica sol and preparation method thereof Download PDFInfo
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Abstract
The invention provides a green environment-friendly polishing silica sol and a preparation method thereof, wherein the silica sol comprises silicon oxide source ethyl orthosilicate, surfactant polyethylene glycol mono-octyl phenyl ether, cosurfactant 4-methyl-2-pentanol, organic solvent cyclohexane, pH regulator potassium tert-butoxide, metal ion chelating agent ethylenediamine tetraacetic acid, bactericide methylisothiazolinone or methylene dimorpholine, and the balance of deionized water, wherein the size of the obtained silica particles is between 10 and 20nm, the viscosity of the silica sol is less than or equal to 10mm 2/s at normal temperature, the pH value is 10.5 to 12.5, and the specific gravity is 1.1 ~ 1.3.3 g/cm 3.
Description
Technical Field
the invention relates to the technical field of polishing silica sol, in particular to green and environment-friendly LED sapphire substrate polishing silica sol and a preparation method thereof.
Background
With the rapid development of optoelectronic technology and the increasing demand of LED optoelectronic product materials, there are many substrate materials that can be used for GaN wafer LEDs, but the number of substrate materials that can be actually used for commercialization is still small, and there are only two kinds of substrate materials, namely sapphire and SiC, and there is no third substrate for the commercial production of GaN LEDs. Compared with sapphire, SiC is a very important substrate material, is a low-resistance material, can be used for manufacturing electrodes, has a lattice constant and a thermal expansion coefficient which are closer to those of a GaN material, is easy to dissolve, has a blue light emitting characteristic, but has the defects that the difference between the thermal expansion coefficient and the GaN is large, cracks of an epitaxial GaN layer are easily caused, the epitaxial GaN layer is not suitable for being used in a large amount, and the price is relatively high. Sapphire substrates are currently the best and most commonly used substrate material.
sapphire crystal (α -a1 2 O 3) is a high-quality optical functional material with high temperature resistance, wear resistance, corrosion resistance and wide light transmission band, has the same hexagonal close-packed type as group iii nitrides, and is an excellent material with a unique combination of physical, mechanical and chemical characteristics in the field of optical communications, sapphire crystal is used not only as a short-wavelength active device but also as a passive device for polarized light in the field of microelectronics, and sapphire can be used as a substrate for a new generation of semiconductor substrate SOI (on-insulator), and due to the excellent blocking effect of sapphire, the operating speed can be faster and the power consumption can be lower.
the conventional CMP is silica sol which is a hard and brittle ceramic material and has very low surface chemical activity, SiO 2 hydrosol is of a double-electronic-layer structure, electrons on the outer layer show negative charges, and the surface of colloidal SiO 2 particles prepared by a condensation method is rich in silicon hydroxyl groups.
however, the silica sol reported in the current domestic patent has the following problems: (1) the particle size is too large, for example, CN106966399A prepares silica sol with large particle size of 105nm-120nm by using seed crystal of 10nm silica, although generally speaking, the higher the concentration of silica, the larger the size is, the more beneficial to increase polishing rate, but it is undeniable that, under the condition of the same silicon content, the hydroxyl number on the surface of silica sol with large particle size is far lower than that on the surface of silica sol with small particle size, and the hydroxyl number is crucial in the polishing process of silica sol, secondly, the preparation method of the invention is silica which is simply grown, because the growth process of silica is complicated and the mechanism is still unclear, in the actual production, silica sol with uniform size is difficult to prepare, and the polishing stability in the CMP process is not good.
CN106700942A discloses a sapphire polishing composition and a preparation method thereof, wherein 0.1-5% of a saccharide is added into a silica sol, the saccharide can effectively inhibit the generation of corrosion pits and can maintain a constant polishing rate, but an extremely important factor, namely the stability and shelf life of the silica sol, is ignored, and the shelf life of the silica sol generally available in the market is more than half a year. In addition, other patent reports also disclose silica sols having grease added to the silica sol to improve the polishing effect.
CN106978088A discloses a method for preparing a silica sol polishing solution, the silica sol prepared by the method comprises 120nm silica sol with particle size and 43-45% of solid content, and 20-30nm silica sol with 43-45% of solid content, and the applicant claims that the polishing rate of the dual-size silica sol is higher, this is not the case in practice, however, because during polishing, large silica particles have more chance of contacting the sapphire substrate surface, are more likely to react, and thus become larger until an equilibrium state of the two solid-solid reactions is reached, the possibility of reaction of small particles is reduced along with the increase of the polishing times, so that the particle size is basically unchanged, that is, the larger and larger particles are irregular, and the smaller particles cannot be fully utilized, which is not favorable for improving the polishing efficiency.
in addition, the polishing silica sol for the LED sapphire substrate is prepared by the same date application of the invention, and comprises a silicon oxide source, ethyl orthosilicate and 5 ~ 40 wt%, a surfactant, polyethylene glycol mono-octyl phenyl ether and 1 ~ 15 wt%, a cosurfactant, 4-methyl-2-pentanol and 1 ~ 1.5.5 wt%, an organic solvent, cyclohexane and 5 ~ 7 wt%, a pH regulator, potassium tert-butoxide, a metal ion chelating agent, ethylene diamine tetraacetic acid and 3 ~ 5 wt%, and the balance of deionized water, wherein the obtained silicon oxide particles have the size of 10-20nm, the viscosity of the silica sol is less than or equal to 10mm 2/s, the pH value is 10.5-12.5, and the specific gravity is 1.1 ~ 1.2g/cm 3.
disclosure of Invention
aiming at one or more problems in the prior art, the invention provides the green environment-friendly polishing silica sol for the LED sapphire substrate, the size of the silica sol particles in the polishing silica sol is uniform, the polishing effect is stable, the particle size after polishing is not deformed, the hardness of the silica particles is moderate, and the sapphire substrate is not broken or scratched in the polishing process, so that the processed sapphire substrate has a smooth surface and low roughness; the service life is long, and the quality guarantee period is more than 2 years; the polishing efficiency is high, and the utilization rate of hydroxyl is high. The water is used as a main solvent, so that the VOC content is low, the environment is protected, and the harm to a human body is small.
The invention provides a green environment-friendly polishing silica sol, which comprises the following components in parts by weight:
Silicon oxide source ethyl orthosilicate, 5 ~ 40 wt.%;
polyethylene glycol mono octyl phenyl ether, 1 ~ 15 wt.%;
cosurfactant 4-methyl-2-pentanol, 1 ~ 1.5.5 wt.%;
cyclohexane, 1 ~ 2 wt.%;
pH regulator: potassium tert-butoxide;
Metal ion chelating agent, ethylenediaminetetraacetic acid, 3 ~ 5 wt.%;
Bactericide is one of methylisothiazolone or methylene dimorpholine, 0.5 ~ 1.5.5 wt.%;
the rest is deionized water, wherein the size of the obtained silicon oxide particles is between 10 and 20nm, the viscosity of the silica sol is less than or equal to 10mm 2/s at normal temperature, the pH value is 10.5 to 12.5, and the specific gravity is 1.1 ~ 1.3.3 g/cm 3.
The invention also provides a preferable formula of the green environment-friendly polishing silica sol, wherein the silica sol comprises the following components in percentage by weight:
silicon oxide source: ethyl orthosilicate, 20 wt.%;
Surfactant (b): polyethylene glycol mono octyl phenyl ether;
cosurfactant: 4-methyl-2-pentanol, 1.25 wt.%;
organic solvent: cyclohexane, 2 wt.%;
pH regulators: potassium tert-butoxide;
Metal ion chelating agent: ethylenediaminetetraacetic acid, 4 wt.%;
and (3) bactericide: one of methylisothiazolone or methylenedimorpholine, 1 wt.%;
The balance being deionized water, wherein the molar ratio of deionized water/polyethylene glycol monooctylphenyl ether is 23, the silica particles obtained have a size of about 17nm, a pH of 12.0, a specific gravity of 1.17 ~ 1.19.19 g/cm 2 and a viscosity of 7.8mm 2/s.
The invention also provides a preparation method of the green environment-friendly polishing silica sol for the LED sapphire substrate, which comprises the following steps of firstly, sequentially adding the polyethylene glycol mono-octyl phenyl ether surfactant, the 4-methyl-2-pentanol auxiliary surfactant and the cyclohexane organic solvent into a reaction kettle, mixing, magnetically stirring for 10 ~ 20min at normal temperature, adding a certain amount of deionized water, continuously and magnetically stirring for 30 ~ 40min to obtain a uniform and stable W/O emulsion, then sequentially adding the ethylene diamine tetraacetic acid metal ion chelating agent, the ethyl orthosilicate silicon oxide source and the deionized water into the emulsion, stirring, slowly adding a proper amount of potassium tert-butoxide to adjust the pH value to 10.5-12.5, and continuously stirring for 4 ~ 5 h to obtain the silica sol which is uniform and stable, has the viscosity of less than or equal to 10mm 2/s and the size of silicon oxide of 10-20nm, and has a milky appearance.
the reaction kettle of the silica sol is a polyethylene plastic barrel, and the polishing silica sol can be directly used or diluted by deionized water by 1-2 times for use.
Advantageous effects
(1) The size of the silica sol particles is uniform, the polishing effect is stable, and the size of the polished particles is not deformed;
(2) The silicon oxide particles have moderate hardness, and are not broken or scratched in the polishing process, so that the surface of the treated sapphire is smooth and has low roughness;
(3) the service life is long, and the quality guarantee period is more than 2 years;
(4) the polishing efficiency is high, and the utilization rate of hydroxyl is high;
(5) green and environment-friendly, and has little harm to the environment and human body.
Detailed Description
The present invention will be described in further detail below with reference to embodiments.
example 1
a green environment-friendly polishing silica sol, comprising:
silicon oxide source: ethyl orthosilicate, 5 wt.%;
surfactant (b): polyethylene glycol mono octyl phenyl ether; 1wt. -%)
cosurfactant: 4-methyl-2-pentanol, 1 wt.%;
Organic solvent: cyclohexane, 1 wt.%;
pH regulators: potassium tert-butoxide;
Metal ion chelating agent: ethylenediaminetetraacetic acid, 3 wt.%;
and (3) bactericide: one of methylisothiazolone or methylenedimorpholine, 0.5 wt.%;
the balance being deionized water.
A preparation method of green environment-friendly polishing silica sol for an LED sapphire substrate comprises the following steps of firstly, sequentially adding polyethylene glycol mono-octyl phenyl ether surfactant, 4-methyl-2-pentanol co-surfactant and cyclohexane organic solvent into a reaction kettle, mixing, magnetically stirring for 10 ~ 20min at normal temperature, adding a certain amount of deionized water, continuously and magnetically stirring for 30 ~ 40min to obtain uniform and stable W/O emulsion, then sequentially adding ethylene diamine tetraacetic acid metal ion chelating agent, ethyl orthosilicate silicon oxide source, bactericide and deionized water into the emulsion, stirring, slowly adding a proper amount of potassium tert-butoxide to adjust the pH value to 10.5-12.5, and continuously stirring for 4 ~ 5 hours to obtain uniform and stable silica sol with milky appearance.
The reaction kettle of the silica sol is a polyethylene plastic barrel, and the polishing silica sol can be directly used or diluted by deionized water by 1-2 times for use.
Example 2
A green environment-friendly polishing silica sol, comprising:
Silicon oxide source: ethyl orthosilicate, 20 wt.%;
surfactant (b): polyethylene glycol mono octyl phenyl ether;
Cosurfactant: 4-methyl-2-pentanol, 1.25 wt.%;
organic solvent: cyclohexane, 2 wt.%;
pH regulators: potassium tert-butoxide;
metal ion chelating agent: ethylenediaminetetraacetic acid, 4 wt.%;
And (3) bactericide: 1wt.% of one of methylisothiazolone or methylenedimorpholine;
the balance of deionized water, wherein the molar ratio of the deionized water to the polyethylene glycol mono-octyl phenyl ether is 23, the size of the obtained silicon oxide particles is 10-20nm, the pH value is 12.0, the polishing rate is 306nm/min, the stability is more than 2 years, the silicon oxide particles are milky white, the roughness is 0.7nm, the specific gravity is 1.17 ~ 1.19.19 g/cm 2, and the viscosity is 7.8mm 2/s.
example 3
A green environment-friendly polishing silica sol, comprising:
silicon oxide source: ethyl orthosilicate, 40 wt.%;
Surfactant (b): polyethylene glycol mono octyl phenyl ether, 15 wt.%;
Cosurfactant: 4-methyl-2-pentanol, 1.5 wt.%;
Organic solvent: cyclohexane, 7 wt.%;
pH regulator: potassium tert-butoxide;
Metal ion chelating agent: ethylenediaminetetraacetic acid, 5wt.%,
and (3) bactericide: 1.5wt.% of one of methylisothiazolone or methylenedimorpholine;
The balance being deionized water.
particle size testing:
during the preparation process, the polyethylene glycol mono-octyl phenyl ether surfactant, the 4-methyl-2-pentanol cosurfactant, the cyclohexane organic solvent, the ethylene diamine tetraacetic acid metal ion chelating agent, the ethyl orthosilicate silicon oxide source, the potassium tert-butoxide and the bactericide are always weighed, different amounts of deionized water are added into the mixture, the mixture is continuously stirred for 4 ~ 5 hours and is kept stand for 48 hours, and uniform, stable and different sizes of silica particle sol emulsion are obtained.
TABLE 1
| deionized water/polyethylene glycol Monooctyl phenyl Ether (molar ratio) | using TEM test, the average size of 100 particles was counted |
| 5 | 103nm |
| 10 | 72nm |
| 15 | 34nm |
| 23 | 17nm |
the size of the unused silica sol particles is 10-20nm, after the sapphire is polished by using the silica sol provided by the invention, the silica sol particles grow to 40-50nm, the silica particles before polishing are spherical, the particle size after polishing is uniform, no shape change occurs, the silica particles are basically not in an ellipsoid shape, no debris is seen, and therefore, the silica particles are judged not to be abraded and broken, and therefore, the part with increased particle size completely comes from a solid-phase compound generated by Al 2 O 3.
TABLE 2 polishing Rate and stability testing
from the above table, it can be seen that, when the polishing silica sol with the silica sol particle size of 10-20nm is used, although the polishing rate is lower than that of the large-size silica sol particles, the roughness of the obtained polished sapphire is optimal, and under the same concentration, the surface of the small-particle silica sol has more abundant hydroxyl groups, which is more beneficial to reducing the usage amount of the silica sol, and the small-particle silica sol has stable polishing effect, the particle size after polishing is moderate, the hardness of the silica particles is moderate, the particles are not broken and scratched in the polishing process, and in addition, the added bactericide inhibits the breeding of bacteria or fungi in the silica sol, thereby improving the stability of the silica sol.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (5)
1. A green environment-friendly polishing silica sol, characterized in that the silica sol comprises:
silicon oxide source ethyl orthosilicate, 5 ~ 40 wt.%;
Polyethylene glycol mono octyl phenyl ether, 1 ~ 15 wt.%;
Cosurfactant 4-methyl-2-pentanol, 1 ~ 1.5.5 wt.%;
cyclohexane, 1 ~ 2 wt.%;
pH regulator: potassium tert-butoxide;
metal ion chelating agent, ethylenediaminetetraacetic acid, 3 ~ 5 wt.%;
bactericide is one of methylisothiazolone or methylene dimorpholine, 0.5 ~ 1.5.5 wt.%;
The balance of deionized water, and the balance of deionized water,
Wherein the molar ratio of the deionized water to the polyethylene glycol mono-octyl phenyl ether is 23, the size of the obtained silica particles is between 10 and 20nm, the viscosity of the silica sol is less than or equal to 10mm 2/s at normal temperature, the pH value is between 10.5 and 12.5, and the specific gravity is 1.1 ~ 1.3.3 g/cm 3.
2. the green environmental polishing silica sol of claim 1, wherein said silica sol comprises:
silicon oxide source: ethyl orthosilicate, 20 wt.%;
surfactant (b): polyethylene glycol mono octyl phenyl ether;
Cosurfactant: 4-methyl-2-pentanol, 1.25 wt.%;
organic solvent: cyclohexane, 2 wt.%;
pH regulator: potassium tert-butoxide;
metal ion chelating agent: ethylenediaminetetraacetic acid, 4 wt.%;
And (3) bactericide: one of methylisothiazolone or methylenedimorpholine, 1 wt.%;
The balance of deionized water, wherein the molar ratio of the deionized water to the polyethylene glycol mono-octyl phenyl ether is 23, the size of the obtained silicon oxide particles is 17nm, the pH value is 12.0, the specific gravity is 1.17 ~ 1.19.19 g/cm 2, and the viscosity is 7.8mm 2/s.
3. the method for preparing green environment-friendly polishing silica sol as claimed in claim 1, wherein polyethylene glycol mono-octyl phenyl ether surfactant, 4-methyl-2-pentanol co-surfactant and cyclohexane organic solvent are sequentially added into a reaction kettle to mix, magnetic stirring is carried out for 10 ~ 20min at normal temperature, a certain amount of deionized water is added, magnetic stirring is continued for 30 ~ 40min to obtain uniform and stable W/O emulsion, ethylene diamine tetraacetic acid metal ion chelating agent, ethyl orthosilicate silicon oxide source, bactericide and deionized water are sequentially added into the emulsion, stirring is carried out, a proper amount of potassium tert-butoxide is slowly added to adjust the pH value to 10.5-12.5, continuous stirring is carried out for 4 ~ 5 hours to obtain silica sol which is uniform and stable, has viscosity of less than or equal to 10mm 2/s and has silica size of 10-20nm, and the appearance is milky white.
4. the method for preparing green environment-friendly polishing silica sol according to claim 3, wherein the reaction kettle of the silica sol is a polyethylene plastic bucket.
5. use of the green environmental polishing silica sol according to any one of claims 1 to 2, wherein the polishing silica sol can be used as it is or after being diluted 1 to 2 times with deionized water.
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