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US3620781A Expired / Lapsed US ⏱️ 0.0 years remaining

Partially stabilized zirconia refractory

Assignee: Didier Werke AG
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Filing: 1969-08-06
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Granted: 1971-11-16
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Expires: 1989-08-06
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Abstract

Abstract Body consisting essentially of ZrO2 and CaO with CaO being 2-5 wt. percent of the body. Microstructure consists essentially of cubic grains collectively constituting volumetrically the major phase, smaller primary monoclinic zirconia grains randomly dispersed substantially at grain boundaries between adjacent cubic grains, and, as a principal new feature effecting increased strength and elasticity properties, extremely finely divided precipitate of monoclinic zirconia dispersed intragrangularly throughout the cubic grains and being substantially smaller than the primary monoclinic zirconia grains. Cubic grains composed essentially of a solid solution of ZrO2 in a compound CaZr4O9. Manufacturing process comprises preparing batch material of prescribed composition, heating the material at firing temperature of at least 1,800* C. that causes sintering or melting of the material, cooling fired material to an annealing temperature of 900*-1,700* C. and maintaining it at the annealing temperature for at least about one day and thereafter continuing cooling of the material. Product is either sintered or fusioncast body. Batch material can be either unfused or fused finely divided particles. Unfused batch can be either unreacted or prereacted raw materials. For optimum density from unreacted raw material batch, it is heated, prior to molding, to prefiring temperature of 900*-1,300* C. for at least about one day. CaO can be provided in batch by heat decomposable compound whose solid decomposition product is substantially all CaO, e.g. calcium acetate monohydrate.

Inventors

  • 👤 Ronald C Garvie

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-02 16:25
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/01; C04B35/48; C04B35/46; C04B35/50

Claims Analysis

Total Claims: 9
Claim 1
Independent Claim 73 words
The body of claim 1 wherein said cubic grains are composed essentially of a solid solution ZrO2 in a compound of the formula CaZr4O9, the average grain size of said primary monoclinic zirconia grains is substantially smaller than the average grain size of said cubic grains, the improvement further comprises said precipitate being vermicular and having an average grain size substantially smaller than the average grain size of said primary monoclinic zirconia grains.
Claim 2
Dependent Claim 148 words
The process of making a partially stabilized zirconia body comprising preparing batch material consisting essentially of, on an oxide basis, ZrO2 and CaO, said CaO being (less than about 6 percent) 2 to 5 percent by weight of said material, heating said material at firing temperature in the range of from (temperature that at least causes sintering) at least 1800* C. to and including temperature that causes melting of said material, and thereafter cooling said material, wherein the improvement comprises (proportioning said CaO with said ZrOby weight of said material, said firing CaO content therein of 2 to 5 percent temperature being at least 1800* C.,) interrupting the cooling of said material at an annealing temperature within a range of from 900* C. to 1700* C. and maintaining said material at said annealing temperature for at least about 1 day, and thereafter continuing said cooling of said material.
Claim 3
Dependent Claim 189 words
The process of making a partially stabilized zirconia body comprising preparing a finely divided batch mixture consisting essentially of monoclinic zirconia and calcia, said calcia being (less than about 6 percent) 2 to 5 percent by weight of said mixture, molding said mixture to form a green body, firing said green body at sintering temperature of at least 1800* C., but below the melting point of said mixture until sintering thereof has been effected and the calcia has combined with part of said zirconia to form a cubic crystalline phase, and thereafter cooling the sintered body, wherein the improvement comprises (proportioning said calcia with said zirconia in the preparation of said mixture to yield a CaO content therein of 2 to 5 percent by weight of said mixture, said sintering temperature being at least 1800* C., but below the melting point of said mixture,) interrupting the cooling of said sintered body at an annealing temperature within a range of from 900* C. to 1700* C. and maintaining said sintered body at said annealing temperature for at least about 1 day, and thereafter continuing said cooling of said sintered body.
Claim 4
Dependent Claim 20 words
The process of claim 3 wherein said sintering temperature is within the range of from 1850* C. to 1950* C.
Claim 5
Dependent Claim 20 words
The process of claim 3 wherein said annealing temperature is within the range of from 1250* C. to 1350* C.
Claim 6
Dependent Claim 23 words
The process of claim 3 wherein said calcia is provided by a heat decomposable compound whose solid decomposition product is substantially all CaO.
Claim 7
Dependent Claim 19 words
The process of claim 3 wherein said CaO content is 3 to 4 percent by weight of said mixture.
Claim 8
Dependent Claim 42 words
The process of claim 3 wherein the improvement further comprises, prior to said molding thereof, heating said mixture to a prefiring temperature within a range of 900* C. to 1300* C. for at least about 1 day and thereafter cooling said mixture.
Claim 9
Dependent Claim 20 words
The process of claim 9 wherein said prefiring temperature is within the range of from 1050* C. to 1150* C.

References Cited (Backward Citations)

US2335325A Cited
US2937102A Cited
US3175919A Cited
US3522064A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1974-11-15 1975-05-17 1975-11-16 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1978-11-15 1979-05-17 1979-11-16 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1982-11-15 1983-05-17 1983-11-16 $7700.00 Window Closed / Lapsed

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