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US4639356A Expired / Lapsed US ⏱️ 0.0 years remaining

High technology ceramics with partially stabilized zirconia

Assignee: Wyeth Holdings LLC
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Filing: 1985-11-05
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Granted: 1987-01-27
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Expires: 2005-11-05
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Abstract

Abstract A process for making a fully or a partially stabilized zirconia is disclosed. The process comprises making an aqueous solution of zirconium sulfate in admixture with an inorganic or organic water soluble salt of one or more metals selected from the group consisting of Be, Mg, Ca, Sr, Ba, Ra, Sc, Y, La, Ac, Ce, Hf, Th and Al. The aqueous solution is atomized into a solvent at least partially miscible with water with the solvent being agitated during the addition of the solution. The coprecipitated metal salt formed is separated from the solvent, washed with inert solvent or solvents, dried, and calcined.

Inventors

  • 👤 Michael P. O'Toole
  • 👤 Roger J. Card

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 18:16
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/01; C04B35/48; C04B35/486; B; B82; B82Y; B82Y30/00; C01; C01G; C01G25/00; C01G25/02; C01P; C01P2002/00; C01P2002/50; C01P2002/52; C01P2004/00; C01P2004/30; C01P2004/32; C01P2004/60; C01P2004/64

Claims Analysis

Total Claims: 26
Claim 1
Independent Claim 172 words
A process for making a fully or a partially stabilized zirconia comprising: (a) making an aqueous solution of zirconium sulfate in admixture with an inorganic or organic water soluble salt of one or more metals selected from the group consisting of Be, Mg, Ca, Sr, Ba, Ra, Sc, Y, La, Ac, Ce, Th, and Al, said organic salt having from about 1 to about 20 carbon atoms; (b) atomizing said solution into a solvent at least partially miscible with water, said solvent present in an amount of at least 3 times the volume of said solution wherein the ratio of said solvent to said solution is about 3:1 to about 50:1, based on volume, said solvent being agitated during the addition of said solution, forming a coprecipitated metal salt; (c) separating the coprecipitated metal salt from said solvent by filtration; (d) washing the coprecipitated metal salt filtrate with an inert solvent or solvents; (e) drying the washed filtrate; and (f) calcining the dried filtrate in a flowing gas or mixture of gases.
Claim 2
Dependent Claim 172 words
A process for making a fully or a partially stabilized zirconia comprising: (a) making an aqueous solution of zirconium sulfate in admixture with an inorganic or organic water soluble salt of one or more metals selected from the group consisting of Be, Mg, Ca, Sr, Ba, Ra, Sc, Y, La, Ac, Ce, Th, and Al, said organic salt having from about 1 to about 20 carbon atoms; (b) atomizing said solution into a solvent at least partially miscible with water, said solvent present in an amount of at least 3 times the volume of said solution wherein the ratio of said solvent to said solution is about 3:1 to about 50:1, based on volume, said solvent being agitated during the addition of said solution, forming a coprecipitated metal salt; (c) separating the coprecipitated metal salt from said solvent by filtration; (d) washing the coprecipitated metal salt filtrate with an inert solvent or solvents; (e) drying the washed filtrate; and (f) calcining the dried filtrate in a flowing gas or mixture of gases.
Claim 3
Dependent Claim 32 words
A process of claim 1 wherein deionized, distilled, or millipore filtered water is used for said solution of (a) and wherein said coprecipitated metal salt is separated from said solvent by filtration.
Claim 4
Dependent Claim 103 words
A process of claim 1 wherein said solution of (a) is made by: (i) dissolving said zirconium sulfate in deionized, distilled or millipore filtered water to form a zirconium sulfate solution; (ii) filtering said solution of (i) through a filter having pore sizes of about 0.2 to about 3 μm; (iii) dissolving said organic or inorganic salt in deionized, distilled or millipore filtered water to form a salt solution; (iv) filtering said solution of (iii) through a filter having pore sizes of about 0.2 to about 3 μm; (v) mixing together said solutions of (ii) and (iv) to form said solution of (a).
Claim 5
Dependent Claim 31 words
A process of claim 1 wherein said solution of (a) has about 1 to about 2.5 moles/liter of zirconium sulfate and about 0.01 to about 0.5 moles/liter of said metal salt.
Claim 6
Dependent Claim 28 words
A process of claim 1 wherein said solution of (a) is filtered through a filter having a pore size of about 0.2 to about 3 μm before atomizing.
Claim 7
Dependent Claim 16 words
A process of claim 1 wherein said atomizing is by a pressure nozzle or ultrasonic nozzle.
Claim 8
Dependent Claim 17 words
A process of claim 1 wherein said solvent to solution ratio is about 5:1 to about 20:1.
Claim 9
Dependent Claim 18 words
A process of claim 1 wherein said solvent is agitated by mechanical stirring, magnetic stirring or by ultrasound.
Claim 10
Dependent Claim 31 words
A process of claim 1 wherein said solvent is selected from the group consisting of alcohols having from about 1 to about 8 carbon atoms and mixtures thereof, acetone, and tetrahydrofuran.
Claim 11
Dependent Claim 23 words
A process of claim 9 wherein said alcohol is selected from the group consisting of methanol, ethanol, propanol, isopropanol, n-butanol, isobutanol, and sec-butanol.
Claim 12
Dependent Claim 25 words
A process of claim 1 having the additional step of adding additional solvent to maintain water to solvent ratio of about 1:3 to about 1:50.
Claim 13
Dependent Claim 13 words
A process of claim 1 wherein said inert solvent of (d) is acetone.
Claim 14
Dependent Claim 27 words
A process of claim 1 wherein said inert solvent of (d) is acetone and toluene individually used sequentially with the first use of the sequence being acetone.
Claim 15
Dependent Claim 20 words
A process of claim 1 wherein said separated coprecipitated metal salt is dried at a temperature of about 120° C.
Claim 16
Dependent Claim 26 words
A process of claim 1 wherein said dried coprecipitated metal salt is calcined at a temperature of about 750° C. utilizing air as the flowing gas.
Claim 17
Dependent Claim 36 words
A process of claim 1 wherein said inorganic salt is selected from the group consisting of oxides, sulfates, chlorides, and nitrates; and said organic salt is selected from the group consisting of: citrates, formates, and acetates.
Claim 18
Dependent Claim 179 words
A process of claim 1 wherein (i) deionized, distilled, or millipore filtered water is utilized for said solution of (a); (ii) said solution of (i) has about 1 to about 2.5 moles/liter of zirconium sulfate and about 0.01 to about 0.5 moles/liter of said metal salt; (iii) said solution of (ii) is filtered through a filter having pore sizes of about 0.2 to about 3 μm before atomizing; (iv) said ratio of said solvent to said solution of (iii) is about 5:1 to about 20:1, said solvent being at least partially miscible with water, said solvent being agitated by mechanical stirring, magnetic stirring or ultrasound, said atomizing being by a pressure or a ultrasonic nozzle; (v) additional solvent is added at a rate to maintain a water to solvent ratio of about 1:5 to about 1:20; (vi) said separated coprecipitated salt is washed with acetone; (vii) said washed coprecipitated metal salt is dried at about 120° C. for about 1 to 2 hours; and (viii) said dried coprecipitated metal salt is calcined at about 750° C. utilizing flowing air.
Claim 19
Dependent Claim 14 words
A process of claim 17 wherein the coprecipitated metal salt is separated by filtration.
Claim 20
Dependent Claim 49 words
A process of claim 17 wherein said solvent is selected from the group consisting of alcohols having from 1 to about 8 carbon atoms and mixtures thereof, chloroform, acetone, and tetrahydrofuran; and the metal salt is selected from the group consisting of oxides, sulfates, chlorides, formates, citrates, and acetates.
Claim 21
Dependent Claim 29 words
A process of claim 19 wherein said metal salt is selected from the group consisting of yttrium sulfates, calcium formates, calcium citrates, magnesium citrates, magnesium formates and magnesium sulfates.
Claim 22
Dependent Claim 18 words
A process of claim 19 wherein said metal salt is a yttrium sulfate and said solvent is ethanol.
Claim 23
Dependent Claim 18 words
A process of claim 19 wherein said metal salt is a yttrium sulfate and said solvent is methanol.
Claim 24
Dependent Claim 18 words
A process of claim 19 wherein said metal salt is a yttrium sulfate and said solvent is isopropanol.
Claim 25
Dependent Claim 26 words
A process of claim 19 wherein said metal salt is a yttrium sulfate and said solvent is selected from the group consisting of n-butanol and acetone.
Claim 26
Dependent Claim 17 words
A process of claim 19 wherein said metal salt is calcium formate and said solvent is isopropanol.

References Cited (Backward Citations)

US3415252A Cited
US4365011A Cited
JPS58176127A Cited
US4501818A Cited
US4520114A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1990-01-26 1990-07-28 1991-01-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1994-01-26 1994-07-28 1995-01-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1998-01-26 1998-07-28 1999-01-27 $7700.00 Window Closed / Lapsed

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