KR20160024455A - Method for controlling the size of sol-gel silica particles by organic solvent addition - Google Patents
Method for controlling the size of sol-gel silica particles by organic solvent addition Download PDFInfo
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- KR20160024455A KR20160024455A KR1020140111191A KR20140111191A KR20160024455A KR 20160024455 A KR20160024455 A KR 20160024455A KR 1020140111191 A KR1020140111191 A KR 1020140111191A KR 20140111191 A KR20140111191 A KR 20140111191A KR 20160024455 A KR20160024455 A KR 20160024455A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
Abstract
The present invention relates to a method for controlling the size of sol-gel silica particles using an organic solvent and a method for controlling the polarity of a mixed solvent by mixing two or more organic solvents in a silica sol having a controlled particle size, Stirring the silane mixture in which the alkoxysilane is added to the mixed solvent; And adding a water-based mixture to the silane mixture to synthesize a silica sol. This is accomplished by a method for controlling the size of sol-gel silica particles using an organic solvent and thereby controlling the particle size of the silica sol. Accordingly, it is possible to control the polarity of the organic solvent, especially the non-polar organic solvent, in the process of preparing the silica nanoparticle, thereby adjusting the size of the silica nanoparticle. It also provides an effect that improves the solubility of the alkoxysilane and the catalyst, including non-alcoholic organic solvents.
Description
The present invention relates to a method for controlling the size of sol-gel silica particles using an organic solvent, and more particularly to a method for controlling the size of particles by controlling the polarity of an organic solvent, The present invention relates to a method of controlling the size of sol-gel silica particles using an organic solvent and to a silica sol having a controlled particle size.
Inorganic materials including silica are excellent in corrosion resistance, chemical resistance, abrasion resistance, heat resistance and electrical characteristics, compared with organic materials such as polymers used for general purposes. In recent years, studies on nanocomposites have been actively carried out, in which polymer and inorganic materials are mixed as needed. Particularly, silica in inorganic materials can be easily prepared by solution process using nano-sized particles by sol- This is the reason why many researches have been done. In order to commercially apply such nano-sized silica particles, it is necessary to control particles of various sizes to meet the purpose.
A conventional technique for controlling the size of silica nanoparticles is disclosed in Korean Patent Application Laid-Open No. 10-2009-0053155, an organic solvent-type silica sol, a method for producing the same, and various techniques. In the above prior art, a high purity silica sol is synthesized by hydrolysis and condensation through an excess amount of water at room temperature using tetravalent alkoxysilane as a silica precursor. The size control of the silica nanoparticles by this method can be carried out by controlling the particle size of the sol-gel silica particles according to the particle-size-controlling theory (GH Bogush et al., J. Coll. Interf. Sci. , v142, p1, 1991). That is, it is understood that when the amount of the basic catalyst is increased, the reaction rate is increased at the early stage and the seeds formed in the early stage of the reaction are accumulated in a short time, resulting in formation of large particles. Also, in the case of increasing the amount of water, since water acts as a reactant of hydrolysis, it is explained that the particle size is increased as a result of the active agglomeration of the seed due to the increase of the initial hydrolysis rate for the same reason.
However, in the prior art known to date, the formation and growth of silica particles according to an organic solvent is not well known. In addition, the silica sol prepared as described in the above document is a form of silica nanoparticles dispersed in water, which limits application to various systems. That is, when the organic solvent is used as the dispersion medium, the mixing property is deteriorated. When the water content and the basic catalyst content are increased to control the particle size of the silica, problems such as lowering the organic mixing property and removing the catalyst by-products are increased .
Therefore, in order to synthesize silica sol from silane, it is necessary to systematically study the change of silica particles according to the property of the mixed organic solvent to be formed, that is, the polarity, by adding an organic solvent as a reaction medium.
Accordingly, an object of the present invention is to provide a method for controlling the size of sol-gel silica particles using an organic solvent capable of adjusting the polarity of the organic solvent and thereby controlling the size of the silica nanoparticles, and to provide a silica sol having a controlled particle size .
Another object of the present invention is to provide a method for controlling the size of sol-gel silica particles using an alkoxysilane and an organic solvent having improved solubility of the catalyst, including a non-alcohol organic solvent, and to provide a silica sol having a controlled particle size .
The above-mentioned object can be accomplished by mixing two or more organic solvents to adjust the polarity of the mixed solvent; Stirring the silane mixture in which the alkoxysilane is added to the mixed solvent; And adding an aqueous mixture to the silane mixture to synthesize a silica sol.
Preferably, the organic solvent is a mixture of an alcohol organic solvent and a non-alcohol organic solvent, and the alcohol organic solvent is selected from the group consisting of methyl alcohol, ethyl alcohol, propyl alcohol, Selected from the group consisting of isopropyl alcohol, butyl alcohol, tert-butyl alcohol, pentyl alcohol, benzyl alcohol, and mixtures thereof. And the non-alcoholic organic solvent is one selected from the group consisting of an aromatic organic solvent, an aliphatic organic solvent, an alicyclic organic solvent, and a mixture thereof.
The aromatic organic solvent may be selected from the group consisting of benzene, toluene, xylene, phenol, benzoic acid, nitrobenzene, naphthalene, naphthol, Wherein the aliphatic organic solvent is selected from the group consisting of anthracene, benzopyrene, salicylic acid, aniline, and mixtures thereof. The aliphatic organic solvent may be at least one selected from the group consisting of pentane, hexane, Methylene formamide, heptane, octane, methyl ethyl ketone, methyl isobutyl ketone, acetone, formamide, N-methyl formamide, N, N-Dimethyl formamide, N, N-Dimethyl acetamide, Dimethyl sulfoxide, Glycerol, Methylcellosolve Methyl cellosolve, ethyl cellosolve, propyl cellosolve, isopropyl cellosolve, Isopropyl cellosolve, butyl cellosolve, butyl carbitol, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, Butylene acetate, ethylene glycol, propylene glycol, and butylene glycol, and mixtures thereof. The alicyclic organic solvent may be at least one selected from the group consisting of cyclo But are not limited to, Cyclohexane, Cyclooctane, Cyclohexanone, Cyclooctanone, Tetrahydrofuran, Tetrahydropyran, Pyridine, N-methylpyrrolidone (N-methyl pyrrolidone), and a mixture thereof.
The organic solvent is preferably a mixture of two or more non-alcohol organic solvents.
Wherein the alkoxysilane is one selected from the group consisting of trivalent alkoxysilane and tetraalkoxysilane and the mixture thereof, and the trivalent alkoxysilane is selected from the group consisting of trimethoxysilane, triethoxysilane, triethoxysilane, tri-n-propoxysilane, triisopropoxysilane, methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, and the like. Wherein the tetraalkoxysilane is one selected from the group consisting of phenyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, and mixtures thereof, and the tetraalkoxysilane is selected from the group consisting of tetramethoxysilane ), Tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilane, tetrabutoxysilane (Tetrabu < (R) > it is preferably one selected from the group consisting of toxysilane, tetraphenoxysilane, tetraacetoxysilane, and mixtures thereof.
Further, the step of stirring the silane mixture is carried out at a temperature of 5 to 100 ° C, more preferably the temperature is 30 to 100 ° C, and the temperature is preferably gradually increased from room temperature to 30 to 100 ° C.
The aqueous mixture is mixed with water and a catalyst, and the catalyst is a basic catalyst. The basic catalyst is selected from the group consisting of ammonium hydroxide, ammonium chloride, methylamine, ethylamine, Propyl amine, isopropyl amine, butyl amine, cyclohexyl amine, dimethyl amine, diethyl amine, trimethyl amine, amine, triethylamine, and mixtures thereof. The water is mixed in an amount of 3 to 10 parts by weight with respect to 100 parts by weight of the mixed solvent, and the catalyst is mixed with 0.1 to 2 parts by weight .
Also, the step of synthesizing the silica sol is performed at a temperature of 5 to 100 ° C, and preferably 10 to 30 parts by weight of the alkoxysilane is added to 100 parts by weight of the mixed solvent.
Another object of the present invention is achieved by a silica sol characterized in that the silica particle size is controlled by mixing two or more organic solvents to control the polarity of the mixed solvent.
According to the structure of the present invention described above, the polarity of the organic solvent, particularly the non-polar organic solvent, can be controlled in the process of preparing the silica nanoparticles, thereby providing the effect of controlling the size of the silica nanoparticles.
It also provides an effect that improves the solubility of the alkoxysilane and the catalyst, including non-alcoholic organic solvents.
FIG. 1 is a flowchart of a method for controlling the size of sol-gel silica particles using an organic solvent according to an embodiment of the present invention,
FIG. 2 is a graph showing the adjustment of the size of silica particles by controlling the polarity through toluene.
FIG. 3 is a graph showing the adjustment of the size of silica particles by controlling the polarity through N-methylformamide.
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, a method for controlling the size of sol-gel silica particles using an organic solvent according to an embodiment of the present invention and a silica sol having a controlled particle size will be described in detail.
As shown in FIG. 1, the polarity of the mixed solvent is first controlled (S1).
A mixed solvent is a mixture of two or more organic solvents, and two or more organic solvents having different polarities are mixed to prepare a mixed solvent having a polarity suitable for the desired silica particle size. If it is necessary to prepare silica particles of various sizes, it is possible to prepare silica particles by mixing organic solvents at various ratios and using mixed solvents, respectively.
The organic solvent to be mixed with the mixed solvent may be at least one alcohol-based organic solvent and at least one non-alcoholic organic solvent. In some cases, the non-alcoholic organic solvent may be mixed with at least two non- To control the polarity of the mixed solvent.
The alcohol-based organic solvent may be selected from the group consisting of methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, butyl alcohol, tert-butyl alcohol alcohol, pentyl alcohol, and benzyl alcohol, and mixtures thereof.
The non-alcoholic organic solvent may be selected from the group consisting of an aromatic organic solvent, an aliphatic organic solvent, an alicyclic organic solvent, and a mixture thereof. The aromatic organic solvent may be selected from the group consisting of benzene, toluene, xylene ), Phenol, benzoic acid, nitrobenzene, naphtalene, naphtol, anthracene, benzopyrene, salicylic acid, and aniline. The aliphatic organic solvent may be at least one selected from the group consisting of pentane, hexane, heptane, octane, methyl ethyl ketone, methyl isobutyl ketone, But are not limited to, methyl isobutyl ketone, acetone, formamide, N-methyl formamide, N, N-dimethyl formamide, N, N - N, N-Dimethyl acetamide, Dimethyl su isopropyl cellosolve, butyl cellosolve, butyl cellosolve, ethyl cellosolve, propyl cellosolve, glycerol, methyl cellosolve, isopropyl cellosolve, butyl cellosolve, Butyl carbitol, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butylacetate, ethylene glycol, Propylene glycol, butylene glycol, and mixtures thereof. The alicyclic organic solvent is preferably selected from the group consisting of cyclohexane, cyclooctane, cyclohexanone, cyclohexanone, Cyclohexanone, Cyclooctanone, Tetrahydrofuran, Tetrahydropyran, Pyridine, N-Methylyl, l pyrrolidone), and a mixture thereof.
The silane mixture in which the alkoxysilane is added to the mixed solvent is stirred (S2).
After forming a silane mixture in which trivalent alkoxysilane or tetraalkoxysilane is added to the mixed solvent, stirring is performed so that the alkoxysilane is uniformly dispersed in the mixed solvent. The stirring temperature is from 5 to 100 캜, more preferably from 30 to 100 캜. When stirring is performed at a temperature higher than room temperature, the temperature is preferably gradually increased from room temperature to a desired temperature. When the stirring temperature is lower than 5 ° C, the solvent may freeze depending on the type of the solvent. If the stirring temperature exceeds 100 ° C, the solvent may evaporate depending on the solvent. Therefore, the temperature at which stirring is performed is most preferably from 5 to 100 캜.
10 to 30 parts by weight of alkoxysilane is added to 100 parts by weight of the mixed solvent. The alkoxysilane may be trivalent alkoxysilane or tetravalent alkoxysilane, or a mixture of the two.
Wherein the trivalent alkoxysilane is selected from the group consisting of trimethoxysilane, triethoxysilane, tri-n-propoxysilane, triisopropoxysilane, methyltrimethoxy A group consisting of methyltrimethoxysilane, methyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, and the like. And mixtures thereof. The tetraalkoxysilane is preferably selected from the group consisting of tetramethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilane, tetraethoxysilane, tetraethoxysilane, A group consisting of tetrabutoxysilane, tetraphenoxysilane, tetraacetoxysilane, and the like; That in the group member selected mixture of 1 being preferred.
And an aqueous mixture is added to synthesize a silica sol (S3).
The silica sol synthesis reaction is initiated by adding an aqueous mixture mixed with water and a catalyst to the silane mixture prepared in step S2. 3 to 10 parts by weight of water and 0.1 to 2 parts by weight of catalyst are mixed with 100 parts by weight of the mixed solvent. Water can be replaced by distilled water. Also, the step of synthesizing silica sol is carried out at 5 to 100 ° C as in step S2.
Wherein the basic catalyst is a basic catalyst and the basic catalyst is selected from the group consisting of ammonium hydroxide, ammonium chloride, methylamine, ethylamine, propylamine, Isopropyl amine, butyl amine, cyclohexyl amine, dimethyl amine, diethyl amine, trimethyl amine and triethyl amine. And a mixture thereof.
In the synthesis reaction, 4-alkoxysilane is taken as an example, 4-alkoxysilane is reacted with 4-moles of water to cause hydrolysis and condensation reaction, and 2 moles of water is generated as a product. Of water is needed. Water is a reactant required for hydrolysis. As the amount of water increases, the reaction rate increases and the particle size generally increases. In general reaction conditions, the hydrolysis reaction by water is very slow, so a basic catalyst is used.
The formation and formation of silica particles by the sol-gel reaction is usually explained by the particle aggregation model, and the initial particle seed formation process environment plays an important role in the size of the finally formed particles do. That is, as the content of water and basic catalyst increases, the initial seed generation rate increases, and thus, the aggregation of seeds occurs rapidly, resulting in an increase in the final particle size.
In the present invention, at least one non-alcohol organic solvent is used as a mixed solvent in which two or more organic solvents are mixed in a method capable of controlling the size of silica particles using an organic solvent. This is because the organic materials including polymers such as silicone resin, polyimide, polyamide, polyamideimide, epoxy, acrylic resin and the like are dissolved in alcohol organic solvent It does not melt well. Therefore, only a minimum amount of water, basic catalyst and alcohol solvent is used in the sol-gel reaction, and the control of the remaining particle size is carried out by using the polarity of the non-alcohol organic solvent. When the polarity of the solvent is low in forming the silica particles, the stability of the seed particles in the initial stage is lowered, resulting in a lot of particle aggregation, resulting in an increase in the size of the final particles. This is confirmed by the following examples.
≪ Example 1 >
Methanol and toluene were mixed in various ratios, and 75 parts by weight of a solvent and 15 parts by weight of tetraethoxysilane were stirred for 30 minutes while raising the temperature to 50 占 폚. Then, an aqueous solution obtained by mixing 3.5 parts by weight of distilled water and 0.4 part by weight of aqueous ammonia, which is a basic catalyst, was added to the mixed solvent, and sufficiently reacted until there was no change in solid silica content. At this time, a solid content of about 7 parts by weight was formed. The particle size of the finally prepared silica sol was measured by a dynamic light scattering method. Toluene is a solvent commonly used as a non-polar solvent and has a very low dielectric constant value of ε = 2.4. Fig. 2 is a graph showing the particle size of the silica sol prepared in this manner. As can be seen from the graph, it was confirmed that the particle size increases as the toluene content as the non-polar solvent increases.
≪ Example 2 >
Methanol and N-methyl formamide were mixed in various ratios, and 75 parts by weight of a solvent and 15 parts by weight of tetraethoxysilane were heated for 30 minutes Lt; / RTI > Then, an aqueous solution obtained by mixing 3.5 parts by weight of distilled water and 0.4 part by weight of aqueous ammonia, which is a basic catalyst, was added to the mixed solvent, and sufficiently reacted until there was no change in solid silica content. At this time, a solid content of about 7 parts by weight was formed. The particle size of the finally prepared silica sol was measured by a dynamic light scattering method. N-methylformamide is a very polar solvent and its solution dielectric constant is very high at ε = 180. FIG. 3 is a graph showing the particle size of the silica sol prepared by this method. As can be seen from the graph, it was confirmed that the particle size decreases as the content of the polar solvent N-methylformamide increases.
Claims (19)
Mixing two or more organic solvents to adjust the polarity of the mixed solvent;
Stirring the silane mixture in which the alkoxysilane is added to the mixed solvent;
And adding an aqueous mixture to the silane mixture to synthesize silica sol.
Wherein the organic solvent is a mixture of an alcohol organic solvent and a non-alcohol organic solvent.
The alcohol-based organic solvent includes,
Methyl alcohol, ethyl alcohol, propyl alcohol, isopropyl alcohol, butyl alcohol, tert-butyl alcohol, pentyl alcohol, Pentyl alcohol, benzyl alcohol, and mixtures thereof. The method for controlling the size of silica particles according to claim 1, wherein the silica particles are selected from the group consisting of benzyl alcohol, pentyl alcohol and benzyl alcohol.
The non-alcoholic organic solvent includes,
Wherein the silica particles are selected from the group consisting of aromatic organic solvents, aliphatic organic solvents, alicyclic organic solvents, and mixtures thereof.
The aromatic organic solvent may be,
Benzene, toluene, xylene, phenol, benzoic acid, nitrobenzene, naphtalene, naphtol, anthracene, benzopyrene, ), Salicylic acid, aniline, and mixtures thereof. The method for controlling the size of silica particles according to claim 1, wherein the silica particles are selected from the group consisting of salicylic acid, aniline and mixtures thereof.
The aliphatic organic solvent may be,
But are not limited to, pentane, hexane, heptane, octane, methyl ethyl ketone, methyl isobutyl ketone, acetone, formamide, N-methyl formamide, N, N-dimethyl formamide, N, N-dimethylacetamide, dimethyl sulfoxide ), Glycerol, methyl cellosolve, ethyl cellosolve, propyl cellosolve, isopropyl cellosolve, butyl cellosolve, butyl cellosolve, Butyl carbitol, methyl acetate, ethyl acetate, propyl acetate, isopropyl acetate, butylacetate, ethylene glycol, propylene glycol, Propylene glycol, and butylene glycol. Wherein the silica particles are selected from the group consisting of silica particles and mixtures thereof.
The alicyclic organic solvent includes,
But are not limited to, cyclohexane, cyclooctane, cyclohexanone, cyclooctanone, tetrahydrofuran, tetrahydropyran, pyridine, N-methylpyrrolidone, (N-methyl pyrrolidone), and a mixture thereof.
Wherein the organic solvent is a mixture of two or more non-alcohol organic solvents.
Wherein the alkoxysilane is one selected from the group consisting of trivalent alkoxysilane and tetraalkoxysilane and a mixture thereof.
The trivalent alkoxysilane may be, for example,
But are not limited to, trimethoxysilane, triethoxysilane, tri-n-propoxysilane, triisopropoxysilane, methyltrimethoxysilane, methyl Selected from the group consisting of Methyltriethoxysilane, Phenyltrimethoxysilane, Phenyltriethoxysilane, 3-Glycidoxypropyltrimethoxysilane, and mixtures thereof. Wherein the size of the silica particles is in the range of from 1 to 10.
The tetravalent alkoxysilane may be, for example,
It is preferable to use one or more of tetraethoxysilane, tetraethoxysilane, tetrapropoxysilane, tetraisopropoxysilane, tetrabutoxysilane, tetraphenoxysilane, tetraethoxysilane, tetraethoxysilane, tetraethoxysilane, tetraethoxysilane, (Tetraacetoxysilane), and mixtures thereof. The method for controlling the size of silica particles according to claim 1, wherein the silica particles are selected from the group consisting of tetraethoxysilane and mixtures thereof.
The step of stirring the silane mixture comprises:
At a temperature of 5 to 100 ° C.
The temperature is between 30 and 100 < 0 > C,
Wherein the temperature is gradually increased from room temperature to 30 to 100 占 폚.
Wherein the water-based mixture is mixed with water and a catalyst.
The catalyst is a basic catalyst,
The basic catalyst may be at least one selected from the group consisting of ammonium hydroxide, ammonium chloride, methylamine, ethylamine, propylamine, isopropylamine, A group consisting of a butyl amine, a cyclohexyl amine, a dimethyl amine, a diethyl amine, a trimethyl amine, and a triethyl amine, Wherein the silica particles are selected from the group consisting of silica particles and silica particles.
Wherein the amount of the water is 3 to 10 parts by weight and the amount of the catalyst is 0.1 to 2 parts by weight based on 100 parts by weight of the mixed solvent.
The step of synthesizing a silica sol comprises:
At a temperature of 5 to 100 ° C.
Wherein 10 to 30 parts by weight of the alkoxysilane is added to 100 parts by weight of the mixed solvent.
Characterized in that the silica particle size is controlled by mixing two or more organic solvents to control the polarity of the mixed solvent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190027091A (en) * | 2017-09-06 | 2019-03-14 | 한국전기연구원 | Process for preparing sol-gel silica particles using alkanolamine catalyst and method for manufacturing coated substrate coated with silica particles the same |
| CN115611286A (en) * | 2021-07-16 | 2023-01-17 | 万华化学集团电子材料有限公司 | Preparation method of peanut-shaped ultra-high-purity silica sol, ultra-high-purity silica sol and application of ultra-high-purity silica sol |
| CN115611287A (en) * | 2021-07-16 | 2023-01-17 | 万华化学集团电子材料有限公司 | Preparation method of ultra-high-purity silica sol with adjustable association degree, ultra-high-purity silica sol and application of ultra-high-purity silica sol |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20190027091A (en) * | 2017-09-06 | 2019-03-14 | 한국전기연구원 | Process for preparing sol-gel silica particles using alkanolamine catalyst and method for manufacturing coated substrate coated with silica particles the same |
| WO2019050163A1 (en) * | 2017-09-06 | 2019-03-14 | 한국전기연구원 | Method for manufacturing sol-gel silica particles using alcohol amine catalyst and method for manufacturing coating substrate coated with silica particles |
| CN115611286A (en) * | 2021-07-16 | 2023-01-17 | 万华化学集团电子材料有限公司 | Preparation method of peanut-shaped ultra-high-purity silica sol, ultra-high-purity silica sol and application of ultra-high-purity silica sol |
| CN115611287A (en) * | 2021-07-16 | 2023-01-17 | 万华化学集团电子材料有限公司 | Preparation method of ultra-high-purity silica sol with adjustable association degree, ultra-high-purity silica sol and application of ultra-high-purity silica sol |
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