US4723978A
Expired / Lapsed
US
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Method for a plasma-treated polysiloxane coating
Assignee: International Business Machines Corp
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Filing: 1985-10-31
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Granted: 1988-02-09
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Expires: 2005-10-31
Abstract
Abstract By hydrolyzing an organoalkoysilane monomer at high concentration in solution to form a silanol, allowing the silanol to age to produce a low molecular weight oligomer, spin-applying the oligomer onto a substrate to form a discrete film of highly associated cyclic oligomer thereon, heat treating the oligomer film to form a modified ladder-type silsesquioxane condensation polymer, and then oxidizing the silsesquioxane in an O2 RIE, an organoglass is formed which presents novel etch properties. The organoglass can be used as an etch-stop layer in a passivation process.
Inventors
- 👤 Donna J. Clodgo
- 👤 Rosemary A. Previti-Kelly
- 👤 Erick G. Walton
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-29 12:41
CPC Classifications
H; H10; H10P; H10P14/00; H10P14/60; H10P14/69; H10P14/692; H10P14/6921; H10P14/6922; H10P14/63; H10P14/6326; H10P14/6342; H10P14/65; H10P14/6516; H10P14/6529; H10P14/6532; H10P14/66; H10P14/665; H10P14/668; H10P14/6681; H10P14/6684; H10P14/6686; H10P14/6926; Y; Y10; Y10S; Y10S438/00; Y10S438/97; Y10S65/00; Y10S65/901
Claims Analysis
Total Claims: 12
Claim 1
Independent Claim
133 words
A method of forming an organoglass insulating layer, comprising the steps of: combining an organoalkoxysilane monomer with an aqueous solvent to form a silanol solution having greater than approximately 1.0 vol. % of organoalkoxysilane; subjecting said silanol to an aging period of at least several hours to promote molecular association and convert said silanol to a low molecular weight oligomer in solution; applying said low molecular weight oligomer to a substrate to form a discrete layer of highly associated cyclic oligomer thereon wherein said discrete layer of highly associated cyclic oligomer undergoes insitu poly condensation; heat treating said substrate to cause at least partial oxidative transformation of said cyclic oligomer film to produce a modified ladder-type silsesquioxane polymer and; treating said modified ladder-type silsesquioxane polymer in an oxygen plasma to form an organoglass.
Claim 2
Independent Claim
133 words
A method of forming an organoglass insulating layer, comprising the steps of: combining an organoalkoxysilane monomer with an aqueous solvent to form a silanol solution having greater than approximately 1.0 vol. % of organoalkoxysilane; subjecting said silanol to an aging period of at least several hours to promote molecular association and convert said silanol to a low molecular weight oligomer in solution; applying said low molecular weight oligomer to a substrate to form a discrete layer of highly associated cyclic oligomer thereon wherein said discrete layer of highly associated cyclic oligomer undergoes insitu poly condensation; heat treating said substrate to cause at least partial oxidative transformation of said cyclic oligomer film to produce a modified ladder-type silsesquioxane polymer and; treating said modified ladder-type silsesquioxane polymer in an oxygen plasma to form an organoglass.
Claim 3
Dependent Claim
24 words
The method as recited in claim 1, wherein said organoalkoysilane is selected from the group consisting of gamma-aminopropyltriethoxysilane, gamma-aminopropylmethyldiethoxysilane, beta-(3,4 epoxycyclohexyl) ethyltrimethoxysilane, and beta-aminoethyl-gamma-aminopropyltriethoxysilane.
Claim 4
Dependent Claim
12 words
The method as recited in claim 2, wherein said organoalkoxysilane comprises gamma-aminopropyltriethoxysilane.
Claim 5
Dependent Claim
21 words
The method of claim 1, wherein said solvent is selected from the group consisting of ethanol, methanol, isopropanol and deionized water.
Claim 6
Dependent Claim
23 words
The method as recited in claim 3, wherein said organoalkoxysilane is mixed with deionized water in a volume ratio of 1:3 of organoalkoxysilane:water.
Claim 7
Dependent Claim
27 words
The method as recited in claim 5, wherein said silanol is heat treated by sequential bake cycles at 160° C., 200° C., 250° C. and 350° C.
Claim 8
Dependent Claim
32 words
The method as recited in claim 6, wherein said oxygen plasma treatment step is carried out for 5 minutes in a O 2 RIE reactor at 500 Watts and 125×10 -6 Torr.
Claim 9
Independent Claim
172 words
A method of forming an organoglass insulating layer on a substrate, comprising the steps of substantially hydrolyzing gamma-aminopropyltriethoxysilane monomer to form a silanol having a concentration of at least 25% of the monomer in solution; subjecting said silanol to an aging period of approximately 24 hours to promote intermolecular association and convert said silanol to a low molecular weight oligomer in solution; spin-applying said low molecular weight oligomer onto a substrate to form a discrete layer of highly-associated cyclic oligomer having a thickness greater than approximately 250 Å thereon; sequentially baking said discrete layer of highly-associated cyclic oligomer to form a modified ladder-type silsesquioxane condensation polymer; and exposing said silsesquioxane to a reactive ion etch in an oxygen atmosphere, the resulting organoglass being substantially etch resistant in reactive ion etches carried out in a 100% O 2 atmosphere, and exhibiting an etch initiation period in reactive ion etches carried out in atmosphere of 25% CF 4 /75% O 2 , said etch initiation period increasing with increased O 2 content above 75%.
Claim 10
Independent Claim
172 words
A method of forming an organoglass insulating layer on a substrate, comprising the steps of substantially hydrolyzing gamma-aminopropyltriethoxysilane monomer to form a silanol having a concentration of at least 25% of the monomer in solution; subjecting said silanol to an aging period of approximately 24 hours to promote intermolecular association and convert said silanol to a low molecular weight oligomer in solution; spin-applying said low molecular weight oligomer onto a substrate to form a discrete layer of highly-associated cyclic oligomer having a thickness greater than approximately 250 Å thereon; sequentially baking said discrete layer of highly-associated cyclic oligomer to form a modified ladder-type silsesquioxane condensation polymer; and exposing said silsesquioxane to a reactive ion etch in an oxygen atmosphere, the resulting organoglass being substantially etch resistant in reactive ion etches carried out in a 100% O 2 atmosphere, and exhibiting an etch initiation period in reactive ion etches carried out in atmosphere of 25% CF 4 /75% O 2 , said etch initiation period increasing with increased O 2 content above 75%.
Claim 11
Dependent Claim
21 words
The method as recited in claim 1 wherein said organoglass has a oxygen:silicon ratio at least equivalent to that of quartz.
Claim 12
Dependent Claim
25 words
The method as recited in claim 1 wherein the molecular weight of said oligomer is in a range up to approximately 4000 g/mole after aging.
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