← Back to Patent Explorer
US5137749A Expired / Lapsed US ⏱️ 0.0 years remaining

Method of forming metal oxide film by using metal alkoxide solution

Assignee: Central Glass Co Ltd
•
Filing: 1990-12-19
•
Granted: 1992-08-11
•
Expires: 2010-12-19
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract The invention relates to a sol-gel method for forming a metal oxide film, e.g. TiO 2 film or TiO 2 -SiO 2 film, on a substrate by applying a solution of at least one metal alkoxide to the substrate to form a sol film on the substrate, drying the sol film to cause it to turn into a gel film by hydrolysis and baking the gel film. According to the invention the viscosity of the metal alkoxide solution is adequately increased, preferably to 3-30 cP at 20° C., by the addition of a combination of a hydroxypropyl cellulose of which 2 wt % aqueous solution has a viscosity of 150-400 cP at 20° C. and another hydroxypropyl cellulose of which 2 wt % aqueous solution has a viscosity of 6-10 cP at 20° C. Metal oxide films formed by this method are free from minute cracks and excellent in optical characteristics and durability. By this method it is possible to form a metal oxide film as thick as about 300 nm without repeating the application of the alkoxide solution to the substrate.

Inventors

  • 👤 Seizi Yamazaki
  • 👤 Kensuke Makita
  • 👤 Yasuo Moriguchi
  • 👤 Katsuto Tanaka

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-06 13:19
CPC Classifications
C; C03; C03C; C03C17/00; C03C17/22; C03C17/23; C03C17/25; C23; C23C; C23C18/00; C23C18/02; C23C18/12; C23C18/1204; C23C18/1208; C23C18/1216; C23C18/1229; C23C18/1245; C23C18/125; C23C18/1254; C03C2217/00; C03C2217/20; C03C2217/21; C03C2217/212; C03C2217/23; C03C2218/00; C03C2218/10; C03C2218/11; C03C2218/113

Claims Analysis

Total Claims: 10
Claim 1
Independent Claim 175 words
A method of forming a metal oxide film on a substrate, the method having the steps of preparing a solution of at least one metal alkoxide, adjusting the viscosity of the alkoxide solution by adding thereto a viscosity adjusting agent, thereafter applying the alkoxide solution to the substrate to form a sol film on the substrate, drying the sol film to cause the sol film to turn into a gel film and baking the gel film to a temperature sufficient to convert the gel film to the metal oxide film, characterized in that said viscosity adjusting agent is a combination of a first hydroxypropyl cellulose of which 2 wt % aqueous solution has a viscosity in the range from 150 to 400 centipoises at 20° C. and a second hydroxypropyl cellulose of which 2 wt % aqueous solution has a viscosity in the range from 6 to 10 centipoises at 20° C., wherein the proportion of said first hydroxypropyl cellulose to said second hydroxypropyl cellulose is in the range from 70:30 to 97:3 by weight.
Claim 2
Independent Claim 175 words
A method of forming a metal oxide film on a substrate, the method having the steps of preparing a solution of at least one metal alkoxide, adjusting the viscosity of the alkoxide solution by adding thereto a viscosity adjusting agent, thereafter applying the alkoxide solution to the substrate to form a sol film on the substrate, drying the sol film to cause the sol film to turn into a gel film and baking the gel film to a temperature sufficient to convert the gel film to the metal oxide film, characterized in that said viscosity adjusting agent is a combination of a first hydroxypropyl cellulose of which 2 wt % aqueous solution has a viscosity in the range from 150 to 400 centipoises at 20° C. and a second hydroxypropyl cellulose of which 2 wt % aqueous solution has a viscosity in the range from 6 to 10 centipoises at 20° C., wherein the proportion of said first hydroxypropyl cellulose to said second hydroxypropyl cellulose is in the range from 70:30 to 97:3 by weight.
Claim 3
Dependent Claim 13 words
A method according to claim 1, wherein said substrate is a glass substrate.
Claim 4
Dependent Claim 17 words
A method according to claim 1, wherein said proportion is in the range from 80:20 to 95:5.
Claim 5
Dependent Claim 33 words
A method according to claim 1, wherein said combination of said first hydroxypropyl cellulose and said second hydroxypropyl cellulose is dissolved in an alcohol before adding the combination to the metal alkoxide solution.
Claim 6
Dependent Claim 32 words
A method according to claim 1, wherein the total amount of said first hydroxypropyl cellulose and said second hydroxypropyl cellulose is from 0.1 to 5 wt % of the metal alkoxide solution.
Claim 7
Dependent Claim 47 words
A method according to claim 1, wherein the total amount of said first hydroxypropyl cellulose and said second hydroxypropyl cellulose is such that after the addition of said combination the metal alkoxide solution has a viscosity in the range from 3 to 30 centipoises at 20° C.
Claim 8
Dependent Claim 26 words
A method according to claim 6, wherein said viscosity of the metal alkoxide solution is in the range from 5 to 15 centipoises at 20° C.
Claim 9
Dependent Claim 15 words
A method according to claim 1, wherein the metal alkoxide solution comprises a titanium alkoxide.
Claim 10
Dependent Claim 16 words
A method according to claim 8, wherein the metal alkoxide solution further comprises a silicon alkoxide.

References Cited (Backward Citations)

US4397666A Cited
US4708821A Cited
GB2208874A Cited
US4943542A Cited
US4874462A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1995-08-11 1996-02-10 1996-08-11 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1999-08-11 2000-02-10 2000-08-11 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2003-08-11 2004-02-10 2004-08-11 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag