US5034246A
Expired / Lapsed
US
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Method for forming tungsten oxide films
Assignee: Motors Liquidation Co
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Filing: 1990-08-15
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Granted: 1991-07-23
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Expires: 2010-08-15
Abstract
Abstract A method is disclosed for forming a tungsten oxide film on a substrate by applying an alkyl amine tungstate compound thereon and removing at least a portion of the alkyl amine tungstate compound to form a tungsten oxide film. In a preferred embodiment, a solution of alkyl amine tungstate compound is formed in a solvent to uniformly apply the alkyl amine tungstate compound; the solvent is removed by evaporation thereby forming a deposit; the deposit is heated for a time and at a temperature sufficient to at least partially pyrolyze the alkyl amine tungstate compound. The alkyl amine tungstate compound desirably may be selected from the group consisting of bis (di-n-octylammonium) tetratungstate, and di (n-octadecylammonium) tetratungstate. Preferably, bis (di-n-octylammonium) tetratungstate is used. The invention also provides tungsten oxide films which include suboxides of tungsten oxides (WO3); which have an average ratio of oxygen atoms to tungsten atoms equal to or less than 3:1; which are denser than films produced from currently known MOD precursor compounds; which have a color gradient, that is, regions of different color; and wherein the regions of color are electrochromic.
Inventors
- 👤 Andrew M. Mance
- 👤 Adolph L. Micheli
- 👤 Shyam P. Maheswari
- 👤 Mohammad A. Habib
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-28 05:17
CPC Classifications
C; C23; C23C; C23C18/00; C23C18/02; C23C18/12; C23C18/1204; C23C18/1208; C23C18/1216; C23C18/06; C23C18/125; C23C18/1279
Claims Analysis
Total Claims: 16
Claim 1
Independent Claim
64 words
A method for forming a tungsten oxide film comprising the steps of: a) applying onto a substrate a solution containing an alkyl amine tungstate compound, b) drying said solution to form a deposit, and c) heating said deposit for a time and at a temperature sufficient to pyrolyze at least a portion of said alkyl amine tungstate compound to form a tungsten oxide film.
Claim 2
Independent Claim
64 words
A method for forming a tungsten oxide film comprising the steps of: a) applying onto a substrate a solution containing an alkyl amine tungstate compound, b) drying said solution to form a deposit, and c) heating said deposit for a time and at a temperature sufficient to pyrolyze at least a portion of said alkyl amine tungstate compound to form a tungsten oxide film.
Claim 3
Dependent Claim
18 words
A method according to claim 1 wherein said alkyl amine tungstate compound comprises an alkyl amine tetratungstate compound.
Claim 4
Dependent Claim
26 words
A method according to claim 1 wherein said alkyl amine tungstate compound is selected from the group consisting of bis (di-n-octylammonium) tetratungstate, and di (n-octadecylammonium) tetratungstate.
Claim 5
Dependent Claim
14 words
A method according to claim 1 wherein said solution comprises a vaporizable organic solvent.
Claim 6
Dependent Claim
16 words
A method according to claim 4 wherein said solvent is a mixture of 2-propanol and xylene.
Claim 7
Dependent Claim
24 words
A method according to claim 1 wherein regions of said deposit are heated while varying said time for each respective one of said regions.
Claim 8
Dependent Claim
24 words
A method according to claim 1 wherein regions of said deposit are heated while varying said temperature for each respective one of said regions.
Claim 9
Dependent Claim
28 words
A method according to claim 1 wherein said solution consists of an organic compound which includes one of the group of boron, silicon, phosphorus, lithium, tantalum, and palladium.
Claim 10
Independent Claim
98 words
A method for forming a tungsten oxide film comprising the steps of: a) applying onto a substrate a solution containing an alkyl amine tungstate compound dissolved in a vaporizable organic solvent, b) vaporizing said solvent from the applied solution to produce a deposit on said substrate composed predominantly of said alkyl amine tungstate compound, and c) heating the deposit in the presence of an oxygen containing atmosphere for a time greater than 5 minutes and at a temperature greater than 450° C. to decompose said alkyl amine tungstate compound to produce a tungsten oxide film having electrochromic characteristics.
Claim 11
Independent Claim
98 words
A method for forming a tungsten oxide film comprising the steps of: a) applying onto a substrate a solution containing an alkyl amine tungstate compound dissolved in a vaporizable organic solvent, b) vaporizing said solvent from the applied solution to produce a deposit on said substrate composed predominantly of said alkyl amine tungstate compound, and c) heating the deposit in the presence of an oxygen containing atmosphere for a time greater than 5 minutes and at a temperature greater than 450° C. to decompose said alkyl amine tungstate compound to produce a tungsten oxide film having electrochromic characteristics.
Claim 12
Dependent Claim
34 words
The method according to claim 9 wherein said temperature is between about 450° C. and 550° C. and said time is between about 5 and 10 minutes, thereby forming a brown tungsten oxide film.
Claim 13
Dependent Claim
48 words
The method according to claim 9 wherein said temperature is between about 550° C. and 700° C. and said time is about 5 minutes, thereby forming a faint yellow to white tungsten oxide film which has a percentage by weight of tungsten and oxygen greater than 99 percent.
Claim 14
Dependent Claim
51 words
The method according to claim 9 wherein said temperature is between about 450° C. and 550° C. and said time is between about 15 and 25 minutes, thereby forming a faint yellow to white tungsten oxide film which as a percentage by weight of tungsten and oxygen greater than 99 percent.
Claim 15
Independent Claim
140 words
A method for forming a tungsten oxide film comprising the steps of: a) applying onto an ITO coated substrate a solution containing an alkyl amine tungstate compound dissolved in 50:50 2-propanol:xylene solvent, b) vaporizing said 50:50 2-propanol:xylene solvent from the applied solution to produce a deposit on said ITO coated substrate composed predominately of said alkyl amine tungstate compound, and c) heating the deposit in the presence of an oxygen containing atmosphere for a time between about 20 and 25 minutes and at a temperature between about 450° C. and 510° C. to decompose said alkyl amine tungstate compound to produce a tungsten oxide film which in a reduced state has a transmittance between 800-1200 nm which is less than 25 percent and which in an oxidized state has a transmittance between 400-1200 nm which is greater than 80 percent.
Claim 16
Independent Claim
140 words
A method for forming a tungsten oxide film comprising the steps of: a) applying onto an ITO coated substrate a solution containing an alkyl amine tungstate compound dissolved in 50:50 2-propanol:xylene solvent, b) vaporizing said 50:50 2-propanol:xylene solvent from the applied solution to produce a deposit on said ITO coated substrate composed predominately of said alkyl amine tungstate compound, and c) heating the deposit in the presence of an oxygen containing atmosphere for a time between about 20 and 25 minutes and at a temperature between about 450° C. and 510° C. to decompose said alkyl amine tungstate compound to produce a tungsten oxide film which in a reduced state has a transmittance between 800-1200 nm which is less than 25 percent and which in an oxidized state has a transmittance between 400-1200 nm which is greater than 80 percent.
References Cited (Backward Citations)
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| 3.5 Years (Year 4) | 1994-07-22 | 1995-01-21 | 1995-07-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1998-07-22 | 1999-01-21 | 1999-07-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2002-07-22 | 2003-01-21 | 2003-07-23 | $7700.00 | Window Closed / Lapsed |