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US3853673A Expired / Lapsed US ⏱️ 0.0 years remaining

Strengthened glass articles and methods using glass precursor ion exchange medium

Assignee: OI Glass Inc
•
Filing: 1973-04-30
•
Granted: 1974-12-10
•
Expires: 1993-04-30
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Abstract

Abstract A strengthened glass article is prepared by applying to the surface of the article a glass precursor that is (A) a clear solution of a hydrolyzable metalloxane that is preferably a metallosiloxane that is capable of being further hydrolyzed to a cross-linked polymetalloxane or polymetallosiloxane or (B) a cross-linked polymetalloxane that is a polymetallosiloxane that has a gel structure, the cross-linked polymetallosiloxane as defined in parts A and B being prepared by reacting a metal alkoxide such as silicon alkoxide, optionally a metal alkoxide such as an aluminum alkoxide and a precursor of an alkali metal oxide such as potassium acetate, the alkali metal ion of the alkali metal oxide being larger than the alkali metal ion in the glass; and maintaining the glass article and the glass precursor at an elevated temperature sufficiently high to provide a compressive stress layer in the glass article to produce the strengthened article.

Inventors

  • 👤 L Levene
  • 👤 I Thomas

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-25 21:01
CPC Classifications
C; C03; C03C; C03C21/00; C03C21/001; C03C21/002; C03C17/00; C03C17/02

Claims Analysis

Total Claims: 45
Claim 1
Independent Claim 45 words
IN A METHOD OF STRENGTHENING A SILICATE GLAS ARTICLE CONTAINING ALKALI METAL IONS IN WHICH THE ALKALI METAL IONS IN THE SURFACELAYER OF THE GLASS ARE REPLACED BY DIFFERENT ALKALI METAL IONS FROM AN EXTERNAL SOURCE AT ELEVATED TEMPERATURES, THE IMPROVEMENT COMPRISING THE STEPS OF:
Claim 2
Dependent Claim 45 words
IN A METHOD OF STRENGTHENING A SILICATE GLAS ARTICLE CONTAINING ALKALI METAL IONS IN WHICH THE ALKALI METAL IONS IN THE SURFACELAYER OF THE GLASS ARE REPLACED BY DIFFERENT ALKALI METAL IONS FROM AN EXTERNAL SOURCE AT ELEVATED TEMPERATURES, THE IMPROVEMENT COMPRISING THE STEPS OF:
Claim 3
Dependent Claim 72 words
APPLYING TO THE SURFACE OF THE GLASS ARTICLE A GLASS PERCURSOR THAT IS (A) A CLEAR SOLUTION OF A SOLUBLE, FURTHER HYDROLYZABLE METALLOSILOXANE THAT IS CAPABLE OF BEING FURTHER HYDROLYZED TO A CROSS-LINKED POLYMETALLOSILOXANE, THE SOLUBLE, FURTHER HYDROLYZABLE METALLOSILOXANE BEING FORMED FROM A SILICON ALKOXIDE AND A PRECURSOR OF AN ALKALI METAL OXIDE, THE ALKALI METAL OF THE ALKALI METAL OXIDE BEING LARGER THAN THE ALKALI METAL ION IN THE GLASS; AND
Claim 4
Dependent Claim 72 words
APPLYING TO THE SURFACE OF THE GLASS ARTICLE A GLASS PERCURSOR THAT IS (A) A CLEAR SOLUTION OF A SOLUBLE, FURTHER HYDROLYZABLE METALLOSILOXANE THAT IS CAPABLE OF BEING FURTHER HYDROLYZED TO A CROSS-LINKED POLYMETALLOSILOXANE, THE SOLUBLE, FURTHER HYDROLYZABLE METALLOSILOXANE BEING FORMED FROM A SILICON ALKOXIDE AND A PRECURSOR OF AN ALKALI METAL OXIDE, THE ALKALI METAL OF THE ALKALI METAL OXIDE BEING LARGER THAN THE ALKALI METAL ION IN THE GLASS; AND
Claim 5
Dependent Claim 92 words
MAINTAINING THE GLASS ARTICLE AND THE GLASS PRECURSOR AT AN ELEVATE TEMPERATURE SUFFICIENTLY HIGH TO CONVERT THE METALLOSILOXANE AS DEFINED IN PART (A) TO A CROSS-LINKED POLYMETALLOSILOXANE GEL STRUCTURE AND A GLASS STRUCTURE CONTAINING THE ALKALI METAL ION THAT IS LARGER THAN THE ALKALI METAL ION IN THE GLASS, THE MAINTAINING OF THE GLASS ARTICLE AT THE ELEVATED TEMPERATURE BEIG FOR A PERIOD OF TIME SUFFICIENT TO FORM A COMPRESSIVE STRESS LAYER IN THE GLASS ARTICLE FROM THE GLASS PRECURSOR FORMED FROM THE CROSS-LINKED POLYMETALLOSILOXANE TO THEREBY PRODUCE A STRENGTHENED GLASS ARTICLE.
Claim 6
Dependent Claim 92 words
MAINTAINING THE GLASS ARTICLE AND THE GLASS PRECURSOR AT AN ELEVATE TEMPERATURE SUFFICIENTLY HIGH TO CONVERT THE METALLOSILOXANE AS DEFINED IN PART (A) TO A CROSS-LINKED POLYMETALLOSILOXANE GEL STRUCTURE AND A GLASS STRUCTURE CONTAINING THE ALKALI METAL ION THAT IS LARGER THAN THE ALKALI METAL ION IN THE GLASS, THE MAINTAINING OF THE GLASS ARTICLE AT THE ELEVATED TEMPERATURE BEIG FOR A PERIOD OF TIME SUFFICIENT TO FORM A COMPRESSIVE STRESS LAYER IN THE GLASS ARTICLE FROM THE GLASS PRECURSOR FORMED FROM THE CROSS-LINKED POLYMETALLOSILOXANE TO THEREBY PRODUCE A STRENGTHENED GLASS ARTICLE.
Claim 7
Dependent Claim 27 words
heating the resultant precursor of step (C) to a temperature and for a time sufficient to convert the same to a homogenous mixture of metal oxides; and
Claim 8
Dependent Claim 27 words
heating the resultant precursor of step (C) to a temperature and for a time sufficient to convert the same to a homogenous mixture of metal oxides; and
Claim 9
Dependent Claim 17 words
converting the glass precursor to a homogenous mixture of metal oxides to form a coating thereon; and
Claim 10
Dependent Claim 17 words
converting the glass precursor to a homogenous mixture of metal oxides to form a coating thereon; and
Claim 11
Dependent Claim 92 words
maintaining the glass article and the glass precursor at an elevated temperature sufficiently high to convert the metallosiloxane as defined in part (A) to a cross-linked polymetallosiloxane gel structure and a glass structure containing the alkali metal ion that is larger than the alkali metal ion in the glass, the maintaining of the glass article at the elevated temperature being for a period of time sufficient to form a compressive stress layer in the glass article from the glass precursor formed from the cross-linked polymetallosiloxane to thereby produce a strengthened glass article.
Claim 12
Dependent Claim 92 words
maintaining the glass article and the glass precursor at an elevated temperature sufficiently high to convert the metallosiloxane as defined in part (A) to a cross-linked polymetallosiloxane gel structure and a glass structure containing the alkali metal ion that is larger than the alkali metal ion in the glass, the maintaining of the glass article at the elevated temperature being for a period of time sufficient to form a compressive stress layer in the glass article from the glass precursor formed from the cross-linked polymetallosiloxane to thereby produce a strengthened glass article.
Claim 13
Dependent Claim 69 words
maintaining the glass article and the glass precursor at an elevated temperature sufficiently high to convert the metallosiloxane having a gel structure to a glass structure, the maintaining of the glass article at the elevated temperature being for a period of time sufficient to form a compressive stress layer in the glass article from the glass precursor that is the cross-linked polymetallosiloxane to thereby produce a strengthened glass article.
Claim 14
Dependent Claim 69 words
maintaining the glass article and the glass precursor at an elevated temperature sufficiently high to convert the metallosiloxane having a gel structure to a glass structure, the maintaining of the glass article at the elevated temperature being for a period of time sufficient to form a compressive stress layer in the glass article from the glass precursor that is the cross-linked polymetallosiloxane to thereby produce a strengthened glass article.
Claim 15
Dependent Claim 46 words
In a method of strengthening a silicate glass article containing alkali metal ions in which the alkali metal ions in the Surface layer of the glass are replaced by different alkali metal ions from an external source at elevated temperatures, the improvement comprising the steps of:
Claim 16
Dependent Claim 46 words
In a method of strengthening a silicate glass article containing alkali metal ions in which the alkali metal ions in the Surface layer of the glass are replaced by different alkali metal ions from an external source at elevated temperatures, the improvement comprising the steps of:
Claim 17
Dependent Claim 32 words
heating the resultant precursor coating of step 1 for a time sufficient to convert the same to a glass coating at a temperature below the annealing temperature of the glass article; and
Claim 18
Dependent Claim 32 words
heating the resultant precursor coating of step 1 for a time sufficient to convert the same to a glass coating at a temperature below the annealing temperature of the glass article; and
Claim 19
Dependent Claim 46 words
In a method of strengthening a silicate glass article containing alkali metal ions in which the alkali metal ions in the surface layer of the glass are replaced by different alkali metal ions from an external source at elevated temperatures, the improvement comprising the steps of:
Claim 20
Dependent Claim 46 words
In a method of strengthening a silicate glass article containing alkali metal ions in which the alkali metal ions in the surface layer of the glass are replaced by different alkali metal ions from an external source at elevated temperatures, the improvement comprising the steps of:
Claim 21
Dependent Claim 60 words
maintaining the glass article and the glass coating thereon at an elevated temperature not substantially above the strain point of the glass article and at an elevated temperature for a period of time sufficient to provide a compressive stress layer in the glass article from the glass coating formed from the glass precursor to thereby produce a strengthened glass article.
Claim 22
Dependent Claim 60 words
maintaining the glass article and the glass coating thereon at an elevated temperature not substantially above the strain point of the glass article and at an elevated temperature for a period of time sufficient to provide a compressive stress layer in the glass article from the glass coating formed from the glass precursor to thereby produce a strengthened glass article.
Claim 23
Dependent Claim 64 words
maintaining the glass article and the glass precursor at an elevated temperature sufficiently high and for a period of time sufficient to provide a compressive stress layer in the glass article from the glass precursor containing the alkali metal oxide that has the alkali metal ion that is larger than the alkali metal ion in the glass to thereby produce a strengthened glass article.
Claim 24
Dependent Claim 64 words
maintaining the glass article and the glass precursor at an elevated temperature sufficiently high and for a period of time sufficient to provide a compressive stress layer in the glass article from the glass precursor containing the alkali metal oxide that has the alkali metal ion that is larger than the alkali metal ion in the glass to thereby produce a strengthened glass article.
Claim 25
Dependent Claim 49 words
heating and maintaining the glass article and the mixture of metal oxides at an elevated temperature sufficiently high and for a period of time to provide a compressive stress surface layer in the glass article from the mixture of the metal oxides to thereby produce a strengthened glass article.
Claim 26
Dependent Claim 49 words
heating and maintaining the glass article and the mixture of metal oxides at an elevated temperature sufficiently high and for a period of time to provide a compressive stress surface layer in the glass article from the mixture of the metal oxides to thereby produce a strengthened glass article.
Claim 27
Independent Claim 48 words
A method for strengthening a silicate glass article containing alkali metal ions in the surface layer thereof which are replaced by different alkali metal ions from an external source and elevated in temperatures not substantially above the strain point of the glass, the method comprising the steps of:
Claim 28
Independent Claim 48 words
A method for strengthening a silicate glass article containing alkali metal ions in the surface layer thereof which are replaced by different alkali metal ions from an external source and elevated in temperatures not substantially above the strain point of the glass, the method comprising the steps of:
Claim 29
Dependent Claim 49 words
A method as defined in claim 4 in which there is also reacted with the metallosiloxane and the additional water in step (C) a metal compound which decomposes to an oxide below about 600*C. the metal compound being an alkali metal compound that decomposes to an alkali metal oxide.
Claim 30
Dependent Claim 18 words
A method as defined in claim 5 in which the alkali metal compound is an alkali metal acetate.
Claim 31
Dependent Claim 16 words
A method as defined in claim 6 in which the alkali metal compound is potassium acetate.
Claim 32
Dependent Claim 16 words
A method as defined in claim 6 in which the alkali metal compound is sodium acetate.
Claim 33
Dependent Claim 16 words
A method as defined in claim 6 in which the alkali metal compound is rubidium acetate.
Claim 34
Dependent Claim 16 words
A method as defined in claim 6 in which the alkali metal compound is cesium acetate.
Claim 35
Dependent Claim 15 words
A method as defined in claim 4 in which the silicon alkoxide is ethyl orthosilicate.
Claim 36
Dependent Claim 15 words
A method as defined in claim 4 in which the silicon alkoxide is methyl orthosilicate.
Claim 37
Dependent Claim 16 words
A method as defined in claim 4 in which the metal alkoxide is aluminum sec. butoxide.
Claim 38
Dependent Claim 21 words
A method as defined in claim 4 in which the precursor of the alkali metal oxide is an alkali metal acetate.
Claim 39
Dependent Claim 16 words
A method as defined in claim 14 in which the alkali metal acetate is sodium acetate.
Claim 40
Dependent Claim 16 words
A method as defined in claim 14 in which the alkali metal acetate is potassium acetate.
Claim 41
Dependent Claim 20 words
A method as defined in claim 4 in which the glass precursor provides a glass of the following approximate composition:
Claim 42
Dependent Claim 18 words
A method as defined in claim 4 in which the silicate glass article has the following approximate composition:
Claim 43
Independent Claim 60 words
A method of strengthening a silicate glass article containing alkali metal ions in which the alkali metal ions of the surface layer are replaced by different alkali metal ions from an external source at elevated temperatures, in which the different alkali metal ions are larger than the alkali metal ions of the surface layer, the method comprising the steps of:
Claim 44
Independent Claim 60 words
A method of strengthening a silicate glass article containing alkali metal ions in which the alkali metal ions of the surface layer are replaced by different alkali metal ions from an external source at elevated temperatures, in which the different alkali metal ions are larger than the alkali metal ions of the surface layer, the method comprising the steps of:
Claim 45
Dependent Claim 10 words
A strengthened glass article made by the method of claim

References Cited (Backward Citations)

US3481726A Cited
US3459673A Cited
US3743491A Cited
US3640093A Cited
US3759683A Cited
US3582395A Cited
US3791808A Cited
US3799754A Cited
US3791809A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1977-12-09 1978-06-10 1978-12-10 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1981-12-09 1982-06-10 1982-12-10 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1985-12-09 1986-06-10 1986-12-10 $7700.00 Window Closed / Lapsed

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