Composition for forming a thin layer with low refractive index, manufacturing method thereof, and manufacturing method of a thin layer with low refractive index

Patent metadata

Field	Value
Publication number	US-9644113-B2
Application number	US-201414261766-A
Country	US
Kind code	B2
Filing date	Apr 25, 2014
Priority date	Apr 25, 2014
Publication date	May 9, 2017
Grant date	May 9, 2017

Abstract

To provide a low refractive index film-forming composition for forming a low refractive index film which has a low refractive index, produces a strong antireflection effect, exhibits excellent adhesiveness with respect to a substrate, and is excellent in water repellency or antifouling properties of the coat surface; a production method of the composition; and a method for forming a low refractive index film. The low refractive index film-forming composition is prepared by generating a hydrolysate of (A) a silicon alkoxide by mixing the (A) silicon alkoxide with (B) water, (C) an inorganic acid or an organic acid, and (D) an organic solvent at a predetermined ratio, and mixing the hydrolysate with (E) silica sol, which is obtained by dispersing fumed silica particles in a liquid medium, at a predetermined ratio.

First claim

The invention claimed is:

1. A low refractive index film-forming composition comprising a hydrolysate of a silicon alkoxide and a silica-sol, wherein the silica-sol comprises silica particles having an average particle size within a range of 37 nm to 50 nm, and wherein the composition is prepared by:
(1) generating a hydrolysate of (A) a silicon alkoxide by:
(i) mixing (A) a silicon alkoxide of Chemical Formula (1):
Si(OR) 4   (1)

wherein R is an alkyl group having 1 to 5 carbon atom,
with (F) a fluoroalkyl group-containing silicon alkoxide of Chemical Formula (2):
CF 2 (CF 2 ) n CH 2 CH 2 Si(OR 1 ) 3   (2)

wherein R 1 is an alkyl group having 1 to 5 carbon atoms, and n is an integer from 0 to 8,
in a mass ratio of 1:0.6 to 1.6 (A:F), and
(ii) mixing the (A) silicon alkoxide and the (F) fluoroalkyl group-containing silicon alkoxide with:
(B) water in a proportion of 0.5 parts by mass to 2.0 parts by mass,
(C) an inorganic acid or an organic acid in a proportion of 0.005 parts by mass to 0.5 parts by mass, and
(D) an organic solvent in a proportion of 1.0 part by mass to 5.0 parts by mass based on 1 part by mass of the (A) silicon alkoxide and (F), wherein the organic solvent is an alcohol, a glycol ether, or a glycol ether acetate,

to form a hydrolysate of the silicon alkoxide,
and (2) mixing the hydrolysate of the silicon alkoxide with (E) a silica sol,

wherein the (E) silica sol is obtained by dispersing fumed silica particles having an average particle size within a range of 37 nm to 50 nm and a specific surface area (BET value) within a range of 50 m 2 /g to 400 m 2 /g in a liquid medium, and wherein the SiO 2 in the (E) silica sol is 1 part by mass to 99 parts by mass of the (E) silica sol when a proportion of SiO 2 in the hydrolysate is regarded as being 1 part by mass.

2. The method for producing a low refractive index film-forming composition of claim 1 comprising,
(1) generating a hydrolysate of (A) a silicon alkoxide by:
(i) mixing (A) a silicon alkoxide of Chemical Formula (1):
Si(OR) 4   (1)

wherein R is an alkyl group having 1 to 5 carbon atom,
with (F) a fluoroalkyl group-containing silicon alkoxide of Chemical Formula (2):
CF 2 (CF 2 ) n CH 2 CH 2 Si(OR 1 ) 3   (2)

wherein R 1 is an alkyl group having 1 to 5 carbon atoms, and n is an integer from 0 to 8,
in a mass ratio of 1:0.6 to 1.6 (A:F), and
(ii) mixing the (A) silicon alkoxide and the (F) fluoroalkyl group-containing silicon alkoxide with:
(B) water in a proportion of 0.5 parts by mass to 2.0 parts by mass,
(C) an inorganic acid or an organic acid in a proportion of 0.005 parts by mass to 0.5 parts by mass, wherein the inorganic or organic acid is oxalic acid, acetic acid, or formic acid, and
(D) an organic solvent in a proportion of 1.0 part by mass to 5.0 parts by mass based on 1 part by mass of the (A) and (F), wherein the organic solvent is an alcohol, a glycol ether, or a glycol ether acetate,

to form a hydrolysate of the silicon alkoxide,
and (2) mixing the hydrolysate of the silicon alkoxide with (E) a silica sol,
wherein the (E) silica sol is obtained by dispersing fumed silica particles having an average particle size within a range of 37 nm to 50 nm and a specific surface area (BET value) within a range of 50 m 2 /g to 400 m 2 /g in a liquid medium, and wherein the SiO 2 in the (E) silica sol is 1 part by mass to 99 parts by mass of the (E) silica sol when a proportion of SiO 2 in the hydrolysate is regarded as being 1 part by mass.

Assignees

• Mitsubishi Materials Corp

Inventors

• Higano Satoko
• Yamasaki Kazuhiko

Classifications

• C03C17/007

  containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase · CPC title

• C03C2217/478

  Silica · CPC title

• C09D183/02 Primary

  Polysilicates · CPC title

• C03C17/009

  Mixtures of organic and inorganic materials, e.g. ormosils and ormocers · CPC title

• C03C2217/732

  made of a single layer · CPC title