Nodular Silica Sol and Method of Producing the Same

Inactive Publication Date: 2010-06-17
JGC CATALYSTS & CHEM LTD
View PDF2 Cites 35 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0044]With the production method according to the present invention, now it is possible to easily obtain a nodular silica sol of particles having heterogeneous forms. When the nodular silica sol as described above is used as a polishing material, an excellent polishing performance is provided. Furthermore, with another production method according to the present invention, it is possible to obtain a highly purified nodular silica sol of particles having heterogeneous forms containing only an extremely small amo

Problems solved by technology

Furthermore, irregularities are generated when aluminum wiring is provided on a silicon wafer and an oxide film of silica or the like as an insulating film is provided, and the irregularities are averaged by polishing the oxide film.
Recently, in association with the needs for size reduction and higher performance of electric and electronic products, a degree of integrated in semiconductor devices has been becoming increasingly higher, but, for instance, when there remain impurities such as Na or K in a separating layer of a transistor, the desired performance may not be realized or some failures may occur.
Especially, when Na is deposited on a surface of a polished semiconductor substrate or of an oxide film, Na having high dispersibility may be trapped in defects of the oxide film or the like.
In this case, even when a circuit is formed on the semiconductor substrate, sometimes an insulation failure or a short circuit may occur, and furthermore the dielectric constant may drop.
With the spherical particles as described above, however, when a portion above the common plane is polished, the metal for a circuit within a wiring trench under concave sections may disadvantageously be polished down to a level under the common plane, and the problem is generally referred to as dishing.
When the dishing (excessive polishing) as described above occurs, there occur such problems as that a thickness of the wiring diminishes and the wiring resistance becomes larger, or that the flatness of an insulating film formed on the polished surface becomes lower, so that there is the need for suppressing the dishing.
In the methods described above, there are the several problems, for instance, that stability of the obtained aqueous silica is not sufficient, or that an alkoxy group (OR group) remains, the density of obtained particles is low, and therefore a sufficient polishing speed can not be obtained when the silica sol is used as a polishing material.
However, since m

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

example 1

Production of Nodular Silica Sol

1-1) Production of a Silicic Acid Solution

[0122]7,000 grams of sodium silicate with the concentration of 7% (water glass No. 3) was passed through a ultra-filtration module (produced by Asahi kasei Corporation: SIP-1013) and the filtered water was recovered to obtain purified water glass. Then deionized water was added to the purified water glass to adjust the silica content to 5%. Then 6,500 grams of water glass with the silica content of 5% was passed through 2.2 litters of the strong acidic cation exchange resin SK1BH (produced by Mitsubishi Chemicals Corporation) by at the space velocity of 3.1 to obtain 6,650 grams of silicic acid solution. The silica content in the obtained silicic acid solution was 4.7%.

1-2) Processing for Highly Purifying a Silicic Acid Solution

[0123]6,650 grams of the silicic acid solution was again passed through 0.4 litters of the strong acidic cation exchange resin SK1BH (produced by Mitsubishi Chemicals Corporation) at th...

example 2

[0140]Deionized water was added to the highly purified silicic acid solution obtained as described in the processes 1-1) and 1-2) in Example 1 to adjust the silica concentration to 2%, and the mixture solution was agitated for 10 minutes without adding ammonia water with the concentration of 1% to keep the pH at 3.8. The mixture solution was kept at the room temperature for 2 hours for aging to obtain 6,650 grams of polymerized silicic acid solution. Viscosity of the silicic acid in the polymerized silicic acid solution was 1.1 mPa·s.

[0141]Ammonia water with the concentration of 15% was added to 1,000 grams of the polymerized silicic acid solution to adjust the pH to 10.4. Then the mixture solution was heated to 95° C. and kept at the temperature for one hour, and then was cooled to the room temperature to obtain a transparent and pale sol. An average diameter of particles in the obtained sol was measured by the dynamic light scattering method to find that the average diameter was 1...

example 3

[0144]Deionized water was added to the highly purified silicic acid solution obtained like in the process 1-1) and 1-2) in Example 1 to adjust the silica content to 2%, and the solution was agitated for 10 minutes. Then 0.4 grams of ammonia water with the concentration of 1% was added to adjust the pH to 4.5, and the mixture solution was kept at the temperature of 80° C. for one hour for aging to obtain 6,650 grams of polymerized silicic acid solution. Viscosity of the silicic acid in the polymerized silicic acid solution was 1.3 mPa·s.

[0145]Ammonia water with the concentration of 15% was added to 1,000 grams of the polymerized silicic acid solution to adjust the pH to 10.4. Then the silicic acid solution was heated to 95° C., and was kept at the temperature for one hour, and then was cooled to the room temperature to obtain a transparent and pale sol. An average diameter of particles in the sol obtained as described above was 33 nm when measured by the dynamic light scattering meth...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

A novel nodular silica sol adapted to use as a polishing material for polishing, for instance, CMP.
The nodular silica sol has a ratio of an average particle diameter (r) measured by the dynamic light scattering method versus a particle diameter (r′) converted to that of an equivalent sphere computed from an average specific surface area measured by means of the nitrogen absorption method (r/r′, referred to as “association ratio”) in a range from 1.2 to 10, the particle diameter (r′) in a range from 5 to 200 nm, and the specific surface area in a range from 13 to 550 m2/g. The nodular silica particles have heterogeneous forms, and contents of Ca and Mg contained in the nodular silica particles are below 1000 ppm against SiO2 respectively.

Description

FIELD OF THE INVENTION[0001]The present invention relates to a method of producing a nodular silica sol which is a preferable polishing material.BACKGROUND OF THE INVENTION[0002]In production of substrates each with a semiconductor integrated circuit thereon, irregularities or steps are generated when a circuit is formed on a silicon wafer with metal such as copper, and therefore metal portions of the circuit are preferentially removed by polishing to remove the irregularities or steps in a surface. Furthermore, irregularities are generated when aluminum wiring is provided on a silicon wafer and an oxide film of silica or the like as an insulating film is provided, and the irregularities are averaged by polishing the oxide film. In the process of polishing a substrate as described above, it is generally required that the polished surface does not include any step nor irregularity and is flat and smooth without any micro blemish or the like, and that the polishing speed is high.[0003...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C01B33/146C09K3/14
CPCC01B33/1435C09K3/1454C01B33/146
Inventor NAKAYAMA, KAZUHIRONAKASHIMA, AKIRANISHIDA, HIROYASUWAKAMIYA, YOSHINORI
Owner JGC CATALYSTS & CHEM LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products