Reflectance reducing film and method of forming same on glass substrate

• US 5,394,269 A
• Filed: 11/12/1993
• Issued: 02/28/1995
• Est. Priority Date: 11/13/1992
• Status: Expired due to Fees

• Current Assignee: Central Glass Company Limited
• Original Assignee: Central Glass Company Limited
• Inventors: Takahashi, Osamu, Arai, Hiroaki, Takamatsu, Atsushi
• Primary Examiner(s): King, Roy V.
• Application Number:
  US08/150,895
• Time in Patent Office: 473 Days
• Field of Search: 427/169, 427/165, 427/164, 427/443.2, 427/226, 65/60.8, 428/428, 359/580, 359/601
• US Class Current: 359/580
• CPC Class Codes: C03C 1/008 for the production of films or coatings
• CPC Class Codes: C03C 17/007 containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
• CPC Class Codes: C03C 17/009 Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
• CPC Class Codes: C03C 2217/213 SiO2
• CPC Class Codes: C03C 2217/425 consisting of a porous layer
• CPC Class Codes: C03C 2217/77 Coatings having a rough surface
• CPC Class Codes: C03C 2218/113 by sol-gel processes
• CPC Class Codes: G02B 1/113 using inorganic layer materials only

Abstract

The invention relates to a reflectance reducing silicon dioxide film formed on a glass substrate by the sol-gel process. To make the film minutely rough, at least two sols are respectively prepared from at least one compound selected from the group consisting of silicon alkoxides and silicon acetylacetonates, such that polymers of the sols have different average molecular weights. Then, the at least two sols are mixed with a solvent so as to prepare a coating solution. The coating solution is applied to the glass substrate so as to form a sol film on the glass substrate. The thus coated glass substrate is heated so as to transform the sol film into a gel film. The gel film which is minutely rough is satisfactory in reflectance reduction.

Claims

1. A method of forming on a glass substrate a silicon dioxide film having a thickness of about 60 to 160 nm and a refractive index of 1.21 to 1.40 and being minutely rough such that the film has micro-pits and/or microscopic land regions, at least one of each micro-pit and each land region having a diameter of 50 to 200 nm, the method comprising the steps of:

(a) preparing at least two sols respectively from at least one compound so as to disperse in said at least two sols at least two polymers of said at least one compound, said at least one compound being selected from the group consisting of silicon alkoxides and silicon acetylacetonates, said at least two polymers having different average molecular weights;

(b) mixing said at least two sols together with a solvent so as to prepare a coating solution;

(c) applying the coating solution to the glass substrate so as to form a sol film on the glass substrate; and

(d) heating the glass substrate and the sol film so as to transform the sol film into a gel film which has a minutely rough surface having micro-pits and/or microscopic and regions.

2. A method according to claim 1, wherein one polymer of said at least two polymers has an average molecular weight ranging from about 800 to about 5,000, and the other at least one polymer of said at least two polymers has an average molecular weight ranging from about 50,000 to about 400,000.

3. A method according to claim 2, wherein said one polymer has an average molecular weight ranging from about 2,000 to about 3,000.

4. A method according to claim 1, wherein at step (b) said one polymer and the other at least one polymer are mixed in the ratio of 1:

10 to 30;

1 by the number of moles reduced to an oxide basis.

5. A method according to claim 1, wherein said solvent is an alcohol solution.

6. A method according to claim 5, wherein said solvent is one selected from the group consisting of isopropyl alcohol and 1-butanol.

7. A method according to claim 1, wherein the glass substrate is heated at step (d) at a temperature not lower than 100°

C.

8. A method according to claim 1, wherein at step (b) the viscosity of the coating solution is adjusted to 1-10 centipoises.

9. A method according to claim 1, wherein at step (b) the concentration of said at least two polymers reduced to an oxide basis in the coating solution is in the range from 0.1 to 10 wt %.

10. A method according to claim 1, wherein at step (c) the coating solution is applied to the glass substrate in an atmosphere having a relative humidity ranging from 40 to 90%.

11. A reflectance reducing silicon dioxide film formed on a glass substrate, the film having a thickness of about 60 to 160 nm and a refractive index of 1.21 to 1.40 and being minutely rough such that the film has micro-pits and/or microscopic land regions, at least one of each micro-pit and each land region having a diameter of 50 to 200 nm, the film being prepared in accordance with the method of claim 1.

12. A method according to claim 1, wherein each land region is defined between adjacent micro-pits.

13. A film according to claim 11, wherein each land region is defined between adjacent micro-pits.

14. A film according to claim 11, wherein micro-pits and land regions are stable when the film is baked at a temperature not lower than 500°

C.