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US4937212A Expired / Lapsed US ⏱️ 0.0 years remaining

Zirconium oxide fibers and process for their preparation

Assignee: 3M Co
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Filing: 1988-12-19
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Granted: 1990-06-26
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Expires: 2008-12-19
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Abstract

Abstract Improved silicon-free, continuous zirconia fibers have diameters greater than 5 micrometers and high tensile strengths. In another aspect, strong, flexible, zirconia fibers are prepared in a process involving the addition of colloidal ZrO 2 particles to a fiber precursor solution.

Inventors

  • 👤 Eric F. Funkenbusch
  • 👤 Tai T. Tran

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 11:07
CPC Classifications
D; D01; D01F; D01F9/00; D01F9/08; C; C04; C04B; C04B35/00; C04B35/622; C04B35/62227; C04B35/62231; C04B35/6225

Claims Analysis

Total Claims: 24
Claim 1
Independent Claim 32 words
A silicon-free, green fiber comprising: (a) crystalline colloidal zirconia particles with diameters in the range of 5 to 200 nm, (b) at least one water soluble zirconium compound, and (c) residual solvent.
Claim 2
Dependent Claim 32 words
A silicon-free, green fiber comprising: (a) crystalline colloidal zirconia particles with diameters in the range of 5 to 200 nm, (b) at least one water soluble zirconium compound, and (c) residual solvent.
Claim 3
Dependent Claim 28 words
The green fiber according to claim 1 wherein said crystalline colloidal zirconia particles comprise 20 to 80 weight percent of the total zirconia equivalent present in said fiber.
Claim 4
Dependent Claim 27 words
The green fiber according to claim 1 wherein said soluble zirconia compound comprises 20 to 80 weight percent of the total zirconia equivalent present in said fiber.
Claim 5
Dependent Claim 15 words
The green fiber according to claim 1 wherein said soluble zirconium compound is zirconyl acetate.
Claim 6
Dependent Claim 12 words
The green fiber according to claim 1 wherein said solvent is water.
Claim 7
Dependent Claim 158 words
The green fiber according to claim 1 further comprising at least one of: (a) a water soluble compound or sol of metals whose oxides are phase change stabilizers for zirconium oxide wherein said metals comprise more than 0 and up to 20 mole percent of the total equivalent moles of zirconia present; (b) at least one water soluble compound or sol of metals whose oxides are grain growth inhibitors for zirconium oxide and wherein said metals comprise more than 0 and up to 20 mole percent of the total equivalent moles of zirconia present; (c) at least one water soluble catalyst or its precursor wherein said catalyst or precursor comprises more than 0 and up to 10 oxide equivalent mole percent of the total equivalent moles of zirconia present; and (d) a water soluble organic polymer wherein said polymer comprises more than 0 and up to 50 wt. percent of the total zirconia mass content of the fiber.
Claim 8
Dependent Claim 34 words
The green fiber according to claim 6 wherein said phase change stabilizer for zirconium oxide is a compound or sol of a metal selected from the group consisting of yttrium, magnesium, calcium, and cerium.
Claim 9
Dependent Claim 14 words
The green fiber according to claim 6 wherein said grain growth inhibitor is aluminum.
Claim 10
Dependent Claim 41 words
The green fiber according to claim 6 wherein said water soluble catalyst or its precursor is selected from the group consisting of chromium, cobalt, copper, iron, nickel, palladium, platinum and vanadium; their respective oxides, and their respective soluble salts or sols.
Claim 11
Dependent Claim 27 words
The green fiber according to claim 6 wherein said water soluble organic polymer is selected from the group consisting of polyethyleneglycol, polyethylene oxide, polyvinylacetate, polyvinylalcohol, and polyvinylpyrrolidone.
Claim 12
Dependent Claim 26 words
The green fiber according to claim 6 wherein said s organic polymer comprises 20 to 40 weight percent of the total zirconia content of said fiber.
Claim 13
Dependent Claim 37 words
A ceramic fiber comprising crystalline zirconia grains having a grain size of at most 1.0 micrometer, said fiber having a diameter in the range of 10 to 60 micrometers and a tensile strength greater than 0.5 GPa.
Claim 14
Dependent Claim 37 words
A ceramic fiber comprising crystalline zirconia grains having a grain size of at most 1.0 micrometer, said fiber having a diameter in the range of 10 to 60 micrometers and a tensile strength greater than 0.5 GPa.
Claim 15
Dependent Claim 9 words
A yarn prepared from the fibers of claim 12.
Claim 16
Dependent Claim 10 words
A knitted fabric prepared from the fibers of claim 13.
Claim 17
Dependent Claim 12 words
A woven or non-woven fabric prepared from the fibers of claim 12.
Claim 18
Dependent Claim 74 words
A process of making a ceramic fiber containing crystalline zirconia grains comprising the steps of: (a) mixing crystalline, colloidal zirconia particles, at least one soluble zirconium compound, and solvent; (b) concentrating said mixture; (c) extruding or blowing said fiber to provide a green fiber; and (d) heating said green fiber to a temperature in the range of 400° to 2000° C. in an oxygen-containing atmosphere to provide said fiber containing crystalline colloidal zirconia particles.
Claim 19
Dependent Claim 74 words
A process of making a ceramic fiber containing crystalline zirconia grains comprising the steps of: (a) mixing crystalline, colloidal zirconia particles, at least one soluble zirconium compound, and solvent; (b) concentrating said mixture; (c) extruding or blowing said fiber to provide a green fiber; and (d) heating said green fiber to a temperature in the range of 400° to 2000° C. in an oxygen-containing atmosphere to provide said fiber containing crystalline colloidal zirconia particles.
Claim 20
Dependent Claim 224 words
A process of making a ceramic fiber containing crystalline zirconia particles comprising the steps of: (a) mixing crystalline, colloidal zirconia particles, at least one soluble zirconium compound, solvent, and at least one of: (1) a water soluble compound or sol of metals whose oxides are phase change stabilizers for zirconium oxide wherein said metals comprise more than 0 and up to 20 mole percent of the total equivalent moles of zirconia present; (2) at least one water soluble compound or sol of metals whose oxides are grain growth inhibitors for zirconium oxide and wherein said metals comprise more than 0 and up to 20 mole percent of the total equivalent moles of zirconia present; (3) at least one water soluble catalyst or its precursor wherein said catalyst or precursor comprises more than 0 and up to 10 oxide equivalent mole percent of the total equivalent moles of zirconia present; and (4) a water soluble organic polymer wherein said polymer comprises more than 0 and up to 50 wt. percent of the total zirconia mass content of the fiber; (b) concentrating said mixture; (c) extruding or blowing said fiber to provide a green fiber; and (d) heating said green fiber to a temperature in the range of 400° to 2000° C. in an oxygen-containing atmosphere to provide said ceramic fiber containing crystalline colloidal zirconia particles.
Claim 21
Dependent Claim 224 words
A process of making a ceramic fiber containing crystalline zirconia particles comprising the steps of: (a) mixing crystalline, colloidal zirconia particles, at least one soluble zirconium compound, solvent, and at least one of: (1) a water soluble compound or sol of metals whose oxides are phase change stabilizers for zirconium oxide wherein said metals comprise more than 0 and up to 20 mole percent of the total equivalent moles of zirconia present; (2) at least one water soluble compound or sol of metals whose oxides are grain growth inhibitors for zirconium oxide and wherein said metals comprise more than 0 and up to 20 mole percent of the total equivalent moles of zirconia present; (3) at least one water soluble catalyst or its precursor wherein said catalyst or precursor comprises more than 0 and up to 10 oxide equivalent mole percent of the total equivalent moles of zirconia present; and (4) a water soluble organic polymer wherein said polymer comprises more than 0 and up to 50 wt. percent of the total zirconia mass content of the fiber; (b) concentrating said mixture; (c) extruding or blowing said fiber to provide a green fiber; and (d) heating said green fiber to a temperature in the range of 400° to 2000° C. in an oxygen-containing atmosphere to provide said ceramic fiber containing crystalline colloidal zirconia particles.
Claim 22
Dependent Claim 23 words
The ceramic fiber according to claim 16 which is a continuous fiber made by the process having a length greater than 1 meter.
Claim 23
Dependent Claim 31 words
A continuous, zirconia fiber prepared according to the process of claim 16, having a diameter in the range of 10 to 60 micrometers, and a tensile strength greater than 0.5 GPa.
Claim 24
Dependent Claim 18 words
The ceramic fiber according to claim 12 having a diameter in the range of 17 to 60 micrometers.

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1993-06-25 1993-12-25 1994-06-26 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1997-06-25 1997-12-25 1998-06-26 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2001-06-25 2001-12-25 2002-06-26 $7700.00 Window Closed / Lapsed

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