US5200237A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Solid-gel precursor solutions and methods for the fabrication of polymetallicsiloxane coating films
Assignee: Associated Universities, Inc.
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Filing: 1991-10-28
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Granted: 1993-04-06
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Expires: 2011-10-28
Abstract
Abstract Solutions and preparation methods necessary for the fabrication of metal oxide cross-linked polysiloxane coating films are disclosed. The films are useful in provide heat resistance against oxidation, wear resistance, thermal insulation, and corrosion resistance of substrates. The sol-gel precursor solution comprises a mixture of a monomeric organoalkoxysilane, a metal alkoxide M(OR)n (wherein M is Ti, Zr, Ge or Al; R is CH3, C2H5 or C3H7; and n is 3 or 4), methanol, water, HCl and NaOH. The invention provides a sol-gel solution, and a method of use thereof, which can be applied and processed at low temperatures (i.e., <1000 DEG C.). The substrate can be coated by immersing it in the above mentioned solution at ambient temperature. The substrate is then withdrawn from the solution. Next, the coated substrate is heated for a time sufficient and at a temperature sufficient to yield a solid coating. The coated substrate is then heated for a time sufficient, and temperature sufficient to produce a polymetallicsiloxane coating.
Inventors
- 👤 Toshifumi Sugama
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-02 16:58
CPC Classifications
C; C09; C09D; C09D183/00; C09D183/14; C08; C08G; C08G77/00; C08G77/48; C08G77/58; C09D4/00
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
80 words
A method of preparing a polymetallicsiloxane coating on a substrate comprising: (a) coating the substrate with a solution comprising a monomeric organoalkoxysilane, containing an imidazole group, a metal alkoxide and a chlorine containing acid in an alcohol/water medium; (b) heating the coated substrate for a time sufficient and at a temperature sufficient to yield a solid coating; and (c) further heating said substrate for a time sufficient and at a temperature sufficient to produce a polymetallisiloxane coating upon said substrate.
Claim 2
Independent Claim
80 words
A method of preparing a polymetallicsiloxane coating on a substrate comprising: (a) coating the substrate with a solution comprising a monomeric organoalkoxysilane, containing an imidazole group, a metal alkoxide and a chlorine containing acid in an alcohol/water medium; (b) heating the coated substrate for a time sufficient and at a temperature sufficient to yield a solid coating; and (c) further heating said substrate for a time sufficient and at a temperature sufficient to produce a polymetallisiloxane coating upon said substrate.
Claim 3
Dependent Claim
19 words
The method of claim 1 wherein the alcohol is selected from the group consisting of methanol, ethanol and propanol.
Claim 4
Dependent Claim
10 words
The method of claim 1, wherein the acid is HCl.
Claim 5
Dependent Claim
44 words
The method of claim 1 wherein the metal alkoxide is of the formula M(OR) n , wherein M is a suitable transition metal; R is CH 3 , C 2 H 5 or C 3 H 7 , and, n is 3 or 4.
Claim 6
Dependent Claim
13 words
The method of claim 4 wherein M is Ti, Ge, Zr or Al.
Claim 7
Dependent Claim
17 words
The method of claim 1 further comprising adjusting the solution to have a pH of about 7.5.
Claim 8
Dependent Claim
15 words
The method of claim 6 wherein said pH is adjusted by adding NaOH or KOH.
Claim 9
Dependent Claim
28 words
The method of claim 1 wherein said step (b) is performed at a temperature of about 100° C. to about 150° C. for a time about 20 hours.
Claim 10
Dependent Claim
29 words
The method of claim 1 wherein said step (c) is performed at a temperature of about 200° C. to about 350° C. for a period of about 20-30 minutes.
Claim 11
Dependent Claim
23 words
The method of claim 1 wherein the monomeric organoalkoxy silane is selected from the group consisting of N(3-(triethoxysilyl) propyl) imidazole and N(3-(triethoxysilyl) propyl)-4,5-dihydroimidazole.
Claim 12
Dependent Claim
44 words
The method of claim 4 wherein the metal alkoxide is selected from the group consisting of Ti(OC 2 H 5 ) 4 , Ti(OC 3 H 2 ) 4 , Zr(OC 3 H 7 ) 4 and Al(OC 3 H 7 ) 3 .
Claim 13
Dependent Claim
10 words
The method of claim 2 wherein the alcohol is methanol.
Claim 14
Dependent Claim
32 words
The method of claim 1 wherein the solution used in step (a) has a ratio of monomeric organoalkoxysilane to metal alkoxide in the range of about 80/20 to about 50/50 by weight.
Claim 15
Dependent Claim
42 words
The method of claim 1 wherein the solution has the following weight percentages of substituents, 18-35 wt % N[3-(triethoxysily)propy]imidazole 9-18 wt % Ti(OC 2 H 5 ) 4 , 21-26 wt % methanol, 13-29 wt % HCl and 14-17 wt % water.
Claim 16
Dependent Claim
43 words
The method of claim 1 wherein the solution has the following weight percentages of substituents 18-35 wt % N[3-triethoxysilyl)propyl]4,5dihydroimidazole monomer, 9-18 wt % Ti(OC 2 H 5 ) 4 , 21-26 wt % methanol, 13-29 wt % HCl and 14-17 wt % water.
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