Silica-based particle dispersion and production method therefor

Patent metadata

Field	Value
Publication number	US-11891307-B2
Application number	US-201917275970-A
Country	US
Kind code	B2
Filing date	Oct 4, 2019
Priority date	Oct 10, 2018
Publication date	Feb 6, 2024
Grant date	Feb 6, 2024

Abstract

A silica-based particle dispersion including a silica-based particle group and a high polishing rate and high surface precision is achieved to a silica-based substrate or a NiP-plated substrate to be polished or the like. A silica-based particle dispersion containing a group including irregularly-shaped and non-irregularly-shaped silica-based particles, wherein the irregularly-shaped silica-based particles each have a plurality of small holes thereinside and a covering silica layer which covers the core, and the silica-based particle group satisfies [1]-[3]. [1] Having an average particle size (D 1 ) of 100-600 nm, and a particle size (D 2 ) of 30-300 nm in terms of specific surface area. [2] An irregular-shape degree D (D=D 1 /D 3 ) represented by the average particle size (D 1 ) and a projected area-equivalent particle size (D 3 ) being in the range of 1.1-5.0. [3] When waveform separation is performed on a volume-reference particle size distribution, a multi-peak distribution in which three or more peaks are detected.

First claim

The invention claimed is:

1. A silica-based particle dispersion comprising a silica-based particle group including irregularly shaped silica-based particles and non-irregularly shaped silica-based particles,
each of the irregularly shaped silica-based particles having a core including a plurality of pores in its interior and a coating silica layer covering the core, the silica-based particle group satisfying [1] to [3] described below:
[1] a weight-average particle size (D 1 ) is 100 to 600 nm, and a particle size in terms of specific surface area (D 2 ) is 30 to 300 nm;
[2] a degree of shape irregularity D (D=D 1 /D 3 ) as expressed by a ratio of the weight-average particle size (D 1 ) to a projected area equivalent particle size (D 3 ) is 1.1 to 5.0; and
[3] a multi-peak distribution in which three or more separation peaks are detected is obtained by waveform separation of a volume-based particle size distribution.

2. The silica-based particle dispersion according to claim 1 , wherein internal pores of the core have an average pore size of 20 nm or less.

3. The silica-based particle dispersion according to claim 1 , wherein the coating silica layer has an average thickness of 1 to 50 nm and contains silica as its main component.

4. The silica-based particle dispersion according to claim 1 , wherein the silica-based particle group has a skewness of −20 to 20 in the volume-based particle size distribution.

5. The silica-based particle dispersion according to claim 1 , wherein a ratio of a volume of a maximum particle component in separation peaks obtained as a result of the waveform separation of the volume-based particle size distribution of the silica-based particle group is 75% or less.

6. The silica-based particle dispersion according to claim 1 , wherein an aspect ratio of a small particle side component in a number-based particle size distribution obtained by SEM image analysis of the silica-based particle group is 1.05 to 5.0.

7. The silica-based particle dispersion according to claim 1 , wherein a coefficient of variation of a particle size in the volume-based particle size distribution of the silica-based particle group is 30% or more.

8. The silica-based particle dispersion according to claim 1 , wherein a smoothness S (S=S 2 /S 1 ) in the silica-based particle group as expressed by a ratio of an area (S 2 ) of a circle equivalent to an average peripheral length according to an image analysis method to an average area (S 1 ) according to the image analysis method is 1.1 to 5.0.

9. The silica-based particle dispersion according to claim 1 , wherein in the volume-based particle size distribution of the silica-based particle group, a ratio Q (Q=Q 2 /Q 1 ) of a volume (Q 2 ) of particles having a size of 0.7 μm or more to a total volume (Q 1 ) is 1.2% or less.

10. A polishing abrasive grain dispersion comprising the silica-based particle dispersion according to claim 1 .

11. A silica-based particle group including irregularly shaped silica-based particles and non-irregularly shaped silica-based particles,
each of the irregularly shaped silica-based particles having a core including a plurality of pores in its interior and a coating silica layer covering the core, the silica-based particle group satisfying [1] to [3] described below:
[1] a weight-average particle size (D 1 ) is 100 to 600 nm, and a particle size in terms of specific surface area (D 2 ) is 30 to 300 nm;
[2] a degree of shape irregularity D (D=D 1 /D 3 ) as expressed by a ratio of the weight-average particle size (D 1 ) to a projected area equivalent particle size (D 3 ) is 1.1 to 5.0; and
[3] a multi-peak distribution in which three or more separation peaks are detected is obtained by waveform separation of a volume-based particle size distribution.

12. A method of producing a silica-based particle group including irregularly shaped silica-based particles and non-irregularly shaped silica-based particles according to claim 11 , the method comprising steps a to c:
(step a) a step which includes subjecting a porous silica-based gel to wet crushing in an alkaline state to obtain a solution containing irregularly shaped porous silica-based gel-including particles;
(step b) a step which includes adding a silicic acid solution to the solution containing the irregularly shaped porous silica-based gel-including particles in the alkaline state and heating the solution to cause the particles to grow with their shape remaining irregular while filling pores between primary particles in the irregularly shaped porous silica-based gel-including particles by a reaction with silicic acid contained in the silicic acid solution, thereby obtaining the irregularly shaped silica-based particles; and
(step c) a step which includes concentrating the silica-based particle group including the irregularly shaped silica-based particles having grown and collecting the concentrated silica-based particle group.

13. The method of producing the silica-based particle group including the irregularly shaped silica-based particles and the non-irregularly shaped silica-based particles according to claim 12 ,
wherein in the step a, the porous silica-based gel having a specific surface area of 300 to 800 m 2 /g is formed into the irregularly shaped porous silica-based gel-including particles having a weight-average particle size of 80 to 550 nm; and
wherein in the step b, the pores between the primary particles in the irregularly shaped porous silica-based gel-including particles are filled by the reaction with the silicic acid to adjust a specific surface area of the irregularly shaped porous silica-based gel-including particles to 100 m 2 /g or less, and to cause the irregularly shaped silica-based particles to grow to have a weight-average particle size of 100 to 600 nm.

14. The method of producing the silica-based particle group including the irregularly shaped silica-based particles and the non-irregularly shaped silica-based particles according to claim 12 ,
wherein in the step a, the porous silica-based gel is subjected to the wet crushing in the alkaline state of pH 8.0 to 11.5 to obtain the solution containing the irregularly shaped porous silica-based gel-including particles;
wherein in the step b, the solution containing the irregularly shaped porous silica-based gel-including particles is adjusted to an SiO 2 concentration of 1 to 10 mass % and heated to a temperature of 60° C. to 170° C., the silicic acid solution is continuously or intermittently added in the alkaline state of pH 9 to 12.5 to fill the pores between the primary particles in the irregularly shaped porous silica-based gel-including particles by the reaction with the silicic acid to reduce the specific surface area of the particles, while causing the particles to grow with their shape remaining irregular; and
wherein in the step c, the solution containing the irregularly shaped silica-based particles having grown is concentrated and the silica-based particle group including the irregularly shaped silica-based particles is collected.

15. The method of producing the silica-based particle group including the irregularly shaped silica-based particles and the non-irregularly shaped silica-based particles according to claim 12 , wherein in the step b, an SiO 2 molarity of the silicic acid solution is 0.5 to 20 moles with respect to an SiO 2 molarity of the solution containing the irregularly shaped porous silica-based gel-including particles.

Assignees

• Jgc Catalysts & Chemicals Ltd

Inventors

• Komatsu Michio
• Nakayama Kazuhiro
• Tanaka Tetsuya
• Tawarazako Yuji
• Mukai Tatsuya
• Miwa Yuki

Classifications

• H10P52/403

  of conductive or resistive materials · CPC title

• C01B33/193 Primary

  of aqueous solutions of silicates · CPC title

• C09G1/02

  containing abrasives or grinding agents {(abrasives as such C09K3/14; polishing of semi-conductors H10P52/40)} · CPC title

• H01L21/3212

  Electricity · mapped topic

• C01P2004/51

  Particles with a specific particle size distribution · CPC title