KR-20260067258-A - METHOD FOR PRODUCING COLLOIDAL SILICA PARTICLES AND COLLOIDAL SILICA PARTICLES PRODUCED USING THE SAME

Abstract

The present invention discloses a method for manufacturing colloidal silica particles and colloidal silica particles manufactured using the same. The present invention comprises the steps of: preparing a mixed solution by mixing an alcohol, an alkali catalyst, and deionized water; preparing a silica precursor solution by adding a silica precursor to the mixed solution; preparing a colloidal silica solution by adding a surfactant containing a carboxyl functional group to the colloidal silica solution; and preparing colloidal silica particles by aging the colloidal silica solution; wherein the step of preparing the colloidal silica particles is characterized in that the colloidal silica particles include bonding by the surfactant through heat treatment.

Inventors

• 박재근
• 김필수
• 전민욱
• 김주연
• 박은하
• 이세희
• 이혜민

Assignees

• 한양대학교 산학협력단

Dates

Publication Date

20260512

Application Date

20241129

Priority Date

20241105

Claims (12)

1. A step of preparing a mixed solution by mixing alcohol, an alkali catalyst, and deionized water; A step of preparing a silica precursor solution by adding a silica precursor to the above mixed solution; and A step of preparing a colloidal silica solution by adding a surfactant containing a carboxyl functional group to the above colloidal silica solution; and A step of preparing colloidal silica particles by ripening the above colloidal silica solution; Includes, A method for manufacturing colloidal silica particles characterized in that the step of manufacturing the colloidal silica particles comprises bonding by the surfactant through heat treatment.
2. In paragraph 1, A method for manufacturing colloidal silica particles, characterized in that the step of manufacturing the above colloidal silica particles involves manufacturing spherical colloidal silica particles using the above surfactant.
3. In paragraph 1, The step of manufacturing the above-mentioned colloidal silica particles is, A method for manufacturing colloidal silica particles characterized in that at least one of the number of carboxyl functional groups and the concentration of the surfactant is controlled according to the molar ratio of deionized water, alkali catalyst, ethanol, and silica.
4. In paragraph 3, The step of manufacturing the above-mentioned colloidal silica particles is, A method for manufacturing colloidal silica particles characterized by controlling at least one of the concentration of the surfactant, the primary abrasive diameter, the colloidal silica abrasive morphology, and the solid loading according to the number of the carboxyl functional groups.
5. In paragraph 3, The step of manufacturing the above-mentioned colloidal silica particles is, A method for manufacturing colloidal silica particles characterized by controlling at least one of the primary abrasive diameter, colloidal silica abrasive morphology, and solid loading according to the concentration of the surfactant.
6. In paragraph 3, A method for manufacturing colloidal silica particles characterized by the number of carboxyl functional groups being 1 to 4.
7. In paragraph 1, The above surfactants are acetic acid, formic acid, gluconic acid, lactic acid, butyric acid, glutamine, threonine, arginine, methionine, lysine, valine, cysteine, glycine, leucine, proline, alanine, isoleucine, picolinic acid, histidine, phenylalanine, serine, tryptophan, asparagine, aminobutyric acid, tyrosine, oxalic acid, succinic acid, A method for preparing colloidal silica particles characterized by comprising at least one of glutaric acid, phthalic acid, itaconic acid, tartaric acid, maleic acid, malic acid, malonic acid, fumaric acid, aspartic acid, glutamic acid, aconitic acid, citric acid, and ethylenediaminetetraacetic acid (EDTA).
8. In paragraph 3, A method for manufacturing colloidal silica particles characterized by the concentration of the surfactant being 0.001 wt% to 10.0 wt%.
9. In paragraph 1, A method for manufacturing colloidal silica particles characterized in that the temperature of the heat treatment is 10℃ to 100℃.
10. In paragraph 1, A method for manufacturing colloidal silica particles, characterized in that the time of the heat treatment is 10 minutes to 20 hours.
11. Comprising colloidal silica particles produced by the method for producing colloidal silica particles according to claim 1, The above colloidal silica particles are characterized by including bonding by a surfactant.
12. In Paragraph 11, Colloidal silica particles characterized by a solid fraction of 1.50 weight% to 2.35 weight% of the above colloidal silica particles.

Description

Method for producing colloidal silica particles and colloidal silica particles produced using the same The present invention relates to a method for manufacturing colloidal silica particles and colloidal silica particles manufactured using the same. More specifically, the present invention relates to a method for manufacturing colloidal silica particles capable of producing spherical colloidal silica particles using a surfactant and colloidal silica particles manufactured using the same. In CMP technology, a wafer to be flattened is placed on a rotating plate, and a pad is brought into contact with the wafer surface. Polishing is performed by rotating both the plate and the pad while supplying a polishing composition between the wafer and the pad. Simultaneously, the surface of the workpiece is polished by the mechanical action between the polishing particles in the CMP polishing composition and the pad surface, while the wafer surface is flattened by a chemical reaction between the compounds in the CMP polishing composition and the surface of the workpiece. Chemical-mechanical polishing compositions and methods for polishing (or planarizing) substrate surfaces are widely known in the relevant art. Polishing compositions (also known as slurries) for polishing dielectrics typically include colloidal silica or ceria abrasives. Those using colloidal silica abrasives typically have a high pH and a high silica concentration (e.g., greater than 12 weight%). Polishing compositions for polishing metal layers (e.g., tungsten or copper) typically include colloidal silica or alumina abrasives as well as various chemical accelerators, such as oxidizers, chelating agents, catalysts, etc. Colloidal silica is a suspension of fine silica particles with a particle size of several nanometers (nm) to several hundred nanometers, and is widely used in many fields such as inorganic fibers, casting, refractories, abrasives, catalysts, and the paper industry. Currently commercially available colloidal silica is manufactured by using water glass as a starting material and then acid-digesting, dialysis, ion-exchange, or gel-digesting the starting material. However, colloidal silica currently on the market or disclosed in various literature has a very high production cost, which acts as a burden of increased costs for application in other fields, making it commercially disadvantageous. Therefore, there is a desire to develop a manufacturing method that can easily produce excellent colloidal silica and reduce manufacturing costs. Furthermore, changes in the particle size of colloidal silica have not been examined in the past. Figure 1 is a schematic diagram illustrating a conventional method for manufacturing colloidal silica. FIG. 2 is a schematic diagram illustrating a method for manufacturing colloidal silica according to an embodiment of the present invention. FIG. 3 is a schematic diagram illustrating colloidal silica according to an embodiment of the present invention. Figure 4 is an image showing the morphology and particle size dependence of a colloidal silica abrasive according to the mole fraction of colloidal silica in a comparative example. Figure 5 is an image illustrating the morphology and particle size dependence of a colloidal silica abrasive according to the mole fraction of colloidal silica according to an example. Figure 6 is an image and graph showing the dependence of the morphology, particle size, and solid content of colloidal silica particles on acetic acid concentration in a synthesis recipe for producing colloidal silica particles of size 20 nm. Figure 7 is an image and graph showing the dependence of the morphology, particle size, and solid content of colloidal silica particles on the concentration of oxalic acid in a synthesis recipe for producing colloidal silica particles of size 20 nm. Figure 8 is an image and graph showing the dependence of the morphology, particle size, and solid content of colloidal silica particles on citric acid concentration in a synthesis recipe for producing colloidal silica particles of size 20 nm. Figure 9 is an image and graph showing the dependence of the morphology, particle size, and solid content of colloidal silica particles on EDTA concentration in a synthesis recipe for producing colloidal silica particles of size 20 nm. Figure 10 is an image and graph showing the dependence of the morphology, particle size, and solid content of colloidal silica particles on acetic acid concentration in a synthesis recipe for producing colloidal silica particles of size 60 nm. Figure 11 is an image and graph showing the dependence of the morphology, particle size, and solid content of colloidal silica particles on the concentration of oxalic acid in a synthesis recipe for producing colloidal silica particles of size 60 nm. Figure 12 is an image and graph showing the dependence of the morphology, particle size, and solid content of colloidal silica particles on citric acid concentration