US4166147A
Expired / Lapsed
US
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Shaped and fired articles of tio2
Assignee: 3M Co
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Filing: 1973-04-16
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Granted: 1979-08-28
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Expires: 1993-04-16
Abstract
Abstract Solid, shaped and fired refractory articles, such as fibers and microspheres, of titanium dioxide are made by shaping, gelling, and firing titania sols. Said fibers can be made by extruding in air a viscous aqueous titania sol, and heating and firing the resulting green fiber to remove water, decompose and volatilize undesired constituents, and form a refractory fiber of polycrystalline titanium dioxide, which is useful, for example, to form refractory fabrics or as reinforcement for composites. Said microspheres can be made by dispersing droplets of an aqueous titania sol in an organic dehydrating liquid, separating the resulting green microspheres from the dehydrating liquid, and heating and firing the green microspheres to form solid refractory microspheres of polycrystalline titanium dioxide, which are useful, for example, in reflective signs or traffic marking surfaces. Said fired fibers and microspheres are preferably transparent to visible light with the titanium dioxide content thereof in its anatase form.
Inventors
- 👤 Roger W. Lange
- 👤 Harold G. Sowman
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 06:49
CPC Classifications
B; B01; B01D; B01D39/00; B01D39/14; B01D39/20; B01J; B01J20/00; B01J20/02; B01J20/06; B01J20/281; B01J20/282; B01J35/00; B01J35/50; B01J35/58; C; C01; C01G; C01G23/00; C01G23/04; C01G23/047; C04; C04B; C04B35/00; C04B35/01; C04B35/46; C04B35/622; C04B35/62227; C04B35/62231; C04B35/62259; C04B35/624; G; G02; G02B; G02B5/00; G02B5/12; G02B5/126; G02B5/128; B01J2220/00; B01J2220/50; B01J2220/54; Y; Y10; Y10T; Y10T428/00; Y10T428/25; Y10T428/256; Y10T428/29; Y10T428/2982; Y10T428/2991; Y10T428/2993; Y10T428/2998
Claims Analysis
Total Claims: 38
Claim 1
Independent Claim
20 words
A transparent, solid, shaped and fired, non-vitreous, homogeneous, continuous refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form.
Claim 2
Dependent Claim
20 words
A transparent, solid, shaped and fired, non-vitreous, homogeneous, continuous refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form.
Claim 3
Dependent Claim
28 words
Transparent, solid, shaped and fired, non-vitreous, homogeneous microspheres having diameters in the range of 1 to 200 microns and comprising predominantly polycrystalline titanium dioxide in its anatase form.
Claim 4
Dependent Claim
28 words
Transparent, solid, shaped and fired, non-vitreous, homogeneous microspheres having diameters in the range of 1 to 200 microns and comprising predominantly polycrystalline titanium dioxide in its anatase form.
Claim 5
Dependent Claim
14 words
The microspheres of claim 2 further comprising one or more of other metal oxide.
Claim 6
Dependent Claim
17 words
A plastic, elastomeric, metallic or ceramic composite with a plurality of microspheres of claim 2 distributed therein.
Claim 7
Dependent Claim
27 words
A solid, shaped and fired, non-vitreous, homogeneous, transparent, continuous refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form, and one or more other metal oxides.
Claim 8
Dependent Claim
27 words
A solid, shaped and fired, non-vitreous, homogeneous, transparent, continuous refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form, and one or more other metal oxides.
Claim 9
Dependent Claim
13 words
The fiber of claim 5, wherein said other metal oxide is chromium oxide.
Claim 10
Dependent Claim
13 words
The fiber of claim 5, wherein said other metal oxide is alumium oxide.
Claim 11
Dependent Claim
13 words
The fiber of claim 5, wherein said other metal oxide is iron oxide.
Claim 12
Dependent Claim
13 words
The fiber of claim 5, wherein said other metal oxide is cobalt oxide.
Claim 13
Dependent Claim
12 words
The fiber of claim 5, wherein said other metal oxide is silica.
Claim 14
Dependent Claim
15 words
The fiber of claim 5, wherein said other metal oxide is chromium oxide and silica.
Claim 15
Dependent Claim
43 words
A solid, shaped and fired, non-vitreous, homogeneous, transparent, continuous, refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form, and one or more other metal oxides selected from the group consisting of chromium oxide, aluminum oxide, iron oxide, cobalt oxide, and silica.
Claim 16
Dependent Claim
43 words
A solid, shaped and fired, non-vitreous, homogeneous, transparent, continuous, refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form, and one or more other metal oxides selected from the group consisting of chromium oxide, aluminum oxide, iron oxide, cobalt oxide, and silica.
Claim 17
Dependent Claim
39 words
A solid, shaped and fired, non-vitreous, homogeneous, transparent, continuous, refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form, and one or more other metal oxides present in an amount sufficient to impart a color to said fiber.
Claim 18
Dependent Claim
39 words
A solid, shaped and fired, non-vitreous, homogeneous, transparent, continuous, refractory fiber comprising predominantly polycrystalline titanium dioxide in its anatase form, and one or more other metal oxides present in an amount sufficient to impart a color to said fiber.
Claim 19
Dependent Claim
31 words
Transparent, solid, shaped and fired, non-vitreous, homogeneous microspheres comprising predominantly polycrystalline titanium dioxide in its anatase form and one or more of the oxides of silicon, chromium, aluminum, iron, and cobalt.
Claim 20
Dependent Claim
31 words
Transparent, solid, shaped and fired, non-vitreous, homogeneous microspheres comprising predominantly polycrystalline titanium dioxide in its anatase form and one or more of the oxides of silicon, chromium, aluminum, iron, and cobalt.
Claim 21
Independent Claim
67 words
A method for forming continuous fibers of solid, transparent refractory comprising predominantly polycrystalline titanium dioxide in its anatase form, which method comprises extruding in air an aqueous acidic titanium oxide sol or aqueous acidic mixture of a titanium compound calcinable in air to titanium dioxide, and heating and firing the resulting amorphous fibers to remove water, acid, organic material, and carbon therefrom and form said continuous fibers.
Claim 22
Independent Claim
67 words
A method for forming continuous fibers of solid, transparent refractory comprising predominantly polycrystalline titanium dioxide in its anatase form, which method comprises extruding in air an aqueous acidic titanium oxide sol or aqueous acidic mixture of a titanium compound calcinable in air to titanium dioxide, and heating and firing the resulting amorphous fibers to remove water, acid, organic material, and carbon therefrom and form said continuous fibers.
Claim 23
Dependent Claim
45 words
A method according to claim 15 wherein the material which is extruded to form said amorphous fibers is a viscous, fiberizable concentrate comprising an aqueous titanium dioxide sol prepared by dispersing in water a gel formed by drying an acidified aqueous mixture of tetraalkyl titanate.
Claim 24
Dependent Claim
20 words
A method according to claim 16 wherein said firing is carried out at a temperature up to about 600° C.
Claim 25
Dependent Claim
43 words
A method according to claim 15 wherein the material which is dispersed as said droplets to form said amorphous microspheres comprises an aqueous titanium dioxide sol prepared by dispersing in water a gel formed by drying an acidified aqueous mixture of tetraalkyl titanate.
Claim 26
Dependent Claim
13 words
The method according to claim 18 wherein said tetraalkyl titanate is tetraisopropyl titanate.
Claim 27
Dependent Claim
12 words
The method of claim 16 wherein said tetraalkyl titanate is tetraisopropyl titanate.
Claim 28
Dependent Claim
45 words
The method of claim 16, wherein said aqueous mixture of said tetraalkyl titanate further comprises a further metal oxide or metal compound which is calcinable in air to its corresponding metal oxide and the resulting shaped and fired refractory article further comprises said metal oxide.
Claim 29
Dependent Claim
11 words
The method of claim 21 wherein said metal oxide is silica.
Claim 30
Dependent Claim
11 words
The method of claim 21 wherein said metal oxide is alumina.
Claim 31
Dependent Claim
11 words
The method of claim 21 wherein said metal oxide is chromia.
Claim 32
Dependent Claim
13 words
The method of claim 21 wherein said metal oxide is chromia and silica.
Claim 33
Independent Claim
72 words
A method for forming refractory microspheres of solid transparent refractory comprising predominantly polycrystalline titanium dioxide in its anatase form, which method comprises dispersing as droplets in an organic dehydrating liquid an aqueous acidic titanium oxide sol or aqueous acidic mixture of a titanium compound calcinable in air to titanium dioxide, recovering the resulting amorphous microspheres from said liquid, and heating and firing said recovered microspheres to convert them to said refractory microspheres.
Claim 34
Independent Claim
72 words
A method for forming refractory microspheres of solid transparent refractory comprising predominantly polycrystalline titanium dioxide in its anatase form, which method comprises dispersing as droplets in an organic dehydrating liquid an aqueous acidic titanium oxide sol or aqueous acidic mixture of a titanium compound calcinable in air to titanium dioxide, recovering the resulting amorphous microspheres from said liquid, and heating and firing said recovered microspheres to convert them to said refractory microspheres.
Claim 35
Dependent Claim
44 words
In a retro-reflective sheeting comprising a monolayer of spherical lense elements and associated reflector adapted in combination therewith to provide retro-reflection, the improvement comprising using as said lense elements transparent, solid, shaped and fired microspheres comprising predominantly polycrystalline titanium dioxide in its anatase form.
Claim 36
Dependent Claim
44 words
In a retro-reflective sheeting comprising a monolayer of spherical lense elements and associated reflector adapted in combination therewith to provide retro-reflection, the improvement comprising using as said lense elements transparent, solid, shaped and fired microspheres comprising predominantly polycrystalline titanium dioxide in its anatase form.
Claim 37
Dependent Claim
30 words
A plastic composite comprising a plastic matrix having dispersed therein a plurality of solid, shaped and fired, non-vitreous, homogeneous, refractory fibers comprising predominantly polycrystalline titanium dioxide in its anatase form.
Claim 38
Dependent Claim
30 words
A plastic composite comprising a plastic matrix having dispersed therein a plurality of solid, shaped and fired, non-vitreous, homogeneous, refractory fibers comprising predominantly polycrystalline titanium dioxide in its anatase form.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1982-08-27 | 1983-02-26 | 1983-08-28 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1986-08-27 | 1987-02-26 | 1987-08-28 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1990-08-27 | 1991-02-26 | 1991-08-28 | $7700.00 | Window Closed / Lapsed |