US20160130184A1 - Sintered ceramic component and a process of forming the same - Google Patents

Sintered ceramic component and a process of forming the same Download PDF

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Publication number
US20160130184A1
US20160130184A1 US14/928,526 US201514928526A US2016130184A1 US 20160130184 A1 US20160130184 A1 US 20160130184A1 US 201514928526 A US201514928526 A US 201514928526A US 2016130184 A1 US2016130184 A1 US 2016130184A1
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Prior art keywords
sintered ceramic
ceramic component
dopant
content
cao
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US14/928,526
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Inventor
Guangyong Lin
Yeshwanth Narendar
Brian C. LaCourse
Wesley R. Robbins
Daniel René Urffer
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Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Saint Gobain Ceramics and Plastics Inc
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Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Saint Gobain Ceramics and Plastics Inc
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Priority to US14/928,526 priority Critical patent/US20160130184A1/en
Assigned to SAINT-GOBAIN CERAMICS & PLASTICS, INC. reassignment SAINT-GOBAIN CERAMICS & PLASTICS, INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: LACOURSE, BRIAN C., ROBBINS, Wesley R., NARENDAR, YESHWANTH, LIN, GUANGYONG
Publication of US20160130184A1 publication Critical patent/US20160130184A1/en
Priority to US15/466,321 priority patent/US10081575B2/en
Assigned to SAINT-GOBAIN CENTRE DE RECHERCHE ET D'ETUDES EUROPEEN reassignment SAINT-GOBAIN CENTRE DE RECHERCHE ET D'ETUDES EUROPEEN ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: URFFER, DANIEL RENE
Abandoned legal-status Critical Current

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    • C04B35/03—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite
    • C04B35/04—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on magnesium oxide, calcium oxide or oxide mixtures derived from dolomite based on magnesium oxide
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Definitions

  • the following is directed to sintered ceramic components and processes of forming the same.
  • Manifolds for solid oxide fuel cells can be made of magnesia-magnesium aluminate spinel ceramics.
  • the starting materials for the ceramics may be commercial grade materials that include impurities that may provide undesired colors for the manifold or potentially may contaminate other components within a solid oxide fuel cell. Improvements in manifold compositions are desired.
  • FIG. 1 includes a dilatometry curve for a comparative sample with a relatively high level of impurities.
  • FIG. 2 includes a dilatometry curve for a comparative sample with a relatively low level of impurities.
  • FIG. 3 includes a dilatometry curve for another comparative sample with a relatively low level of impurities.
  • FIG. 4 includes a dilatometry curve for a CaO-doped sample formed using material having a relatively low level of impurities.
  • FIG. 5 includes a dilatometry curve for a Y 2 O 3 -doped sample formed using material having a relatively low level of impurities.
  • FIG. 6 includes a dilatometry curve for a TiO 2 -doped sample formed using material having a relatively low level of impurities.
  • FIG. 7 includes a dilatometry curve for a co-doped sample formed using material having a relatively low level of impurities.
  • FIG. 8 includes a dilatometry curve for co-doped samples formed using material having a relatively low level of impurities.
  • FIG. 9 includes a plot of relative density as a function of dopant content for different dopants.
  • color space coordinates are expressed in terms of CIE 1976 (CIELAB) coordinates, L*, a*, and b*.
  • dopant is intended to mean a compound that is intentionally added to affect a property of a material to which such compound is added.
  • Group numbers corresponding to columns within the Periodic Table of Elements are based on the IUPAC Periodic Table of Elements, version dated Jan. 21, 2011.
  • An apparatus can include a sintered ceramic component.
  • the apparatus can be an energy generating apparatus that includes one or solid oxide fuel cells or can be a gas-to-liquid membrane system.
  • the sintered ceramic component can be a manifold to provide a gas to or remove a gas from the apparatus or can be another component that is used in conjunction with the solid oxide fuel cell(s) or gas-to-liquid membrane system. Such other component may be used to connect a plurality of solid oxide fuel cells or systems to each other.
  • the sintered ceramic component may include a high purity magnesia magnesium aluminate (“MMA”) that is intentionally doped with one or more impurities to provide good sintering properties, high density, a particular color, if needed or desired, and not have other impurities that could adversely affect the color or adversely interact with other components in the apparatus.
  • MMA magnesia magnesium aluminate
  • the sintered ceramic component can include at least 50 wt. % MgO; at least one desired dopant, wherein each dopant of the at least one desired dopant has a desired dopant content of at least 0.1 wt. %; all impurities are present at a combined impurity content of less than 0.7 wt. %; and a remainder comprising Al 2 O 3 .
  • desired dopant can include CaO, Y 2 O 3 , TiO 2 , another suitable dopant, or any combination thereof.
  • the desired dopant can include SrO, BaO, Sc 2 O 3 , La 2 O 3 , ZrO 2 , HfO 2 , V 2 O 5 , Nb 2 O 5 , Ta 2 O 5 , Mo 2 O 3 , W 2 O 3 , Co 2 O 3 , or any combination thereof.
  • Fe 2 O 3 may be useful as a co-dopant when combined with another dopant, such as CaO.
  • the desired dopant content is at least 0.2 wt. %, at least 0.3 wt. %, at least 0.4 wt.
  • the desired dopant content is no greater than 5 wt. %, no greater than 3 wt. %, no greater than 2 wt. %, or no greater than 1.1 wt. %.
  • the desired dopant content is in a range of 0.2 wt. % to 5 wt. %, 0.3 wt. % to 3 wt. %, 0.4 wt. % to 2 wt. %, or 0.5 wt. % to 1.1 wt. %.
  • the CaO content can be at least 0.2 wt. %, at least 0.3 wt. %, at least 0.4 wt. %, or at least 0.5 wt. %, or may be no greater than 3 wt. %, no greater than 2 wt. %, no greater than 1.5 wt. %, or no greater than 0.95 wt. %.
  • the CaO content is in a range of 0.2 wt. % to 3 wt. %, 0.3 wt. % to 2 wt. %, 0.4 wt. % to 1.5 wt.
  • the Y 2 O 3 content can be at least 0.2 wt. %, at least 0.3 wt. %, at least 0.4 wt. %, or at least 0.5 wt. %, or may be no greater than 3 wt. %, no greater than 2 wt. %, no greater than 1.5 wt. %, or no greater than 0.95 wt. %. In a particular embodiment having Y 2 O 3 , the Y 2 O 3 content is in a range of 0.2 wt. % to 3 wt.
  • the TiO 2 content can be at least 0.2 wt. %, at least 0.3 wt. %, at least 0.4 wt. %, or at least 0.5 wt. %, or may be no greater than 3 wt. %, no greater than 2.5 wt. %, no greater than 2.0 wt. %, or no greater than 1.5 wt. %. In a particular embodiment having TiO 2 , the TiO 2 content is in a range of 0.2 wt. % to 3 wt. %, 0.3 wt. % to 2.5 wt. %, 0.4 wt. % to 2.0 wt. %, or 0.5 wt. % to 1.5 wt. %.
  • some compounds may not be desired dopants.
  • the desired dopant may not include Cr 2 O 3 , NiO, CuO, or any combination thereof.
  • Such compounds may react with MgO or Al 2 O 3 to form a different compound.
  • the ceramic material may be co-doped with a first dopant and a second dopant that is different from the first dopant.
  • the first dopant can include CaO, Y 2 O 3 , or TiO 2
  • the second dopant includes CaO, Y 2 O 3 , TiO 2 , Fe 2 O 3 , SrO, BaO, Sc 2 O 3 , La 2 O 3 , ZrO 2 , HfO 2 , V 2 O 5 , Nb 2 O 5 , Ta 2 O 5 , Mo 2 O 3 , W 2 O 3 , CO 2 O 3 , or any combination thereof.
  • the first dopant is present in the final composition at a higher concentration than the second dopant, and in another embodiment, the first dopant is present in the final composition at a lower concentration than the second dopant.
  • a combination of the first and second dopants is in a range of 1 wt. % to 9 wt. % of the final composition.
  • the sintered ceramic component may include magnesia and alumina.
  • the composition of the sintered ceramic component can be selected to achieve a coefficient of thermal expansion (CTE) to match another component to which the sintered ceramic component may be coupled.
  • CTEs as described herein are the CTEs as measured from 25° C. to 1200° C.
  • the CTE can be at least 9.0 ppm/° C., such as at least 10.3 ppm/° C. or at least 10.6 ppm/° C.
  • the sintered ceramic component may have a CTE of no greater than 13.0 ppm/° C., such as no greater than 12.7 ppm/° C., or no greater than 12.5 ppm/° C.
  • the sintered ceramic component can have a CTE in a range of 9.0 ppm/° C. to 13.0 ppm/° C., 10.3 ppm/° C. to 12.7 ppm/° C., or 10.6 ppm/° C. to 12.5 ppm/° C.
  • the CTE of the sintered ceramic component can match closely to that of the material to be coupled.
  • the sintered having a CTE in a range of 11.0 ppm/° C. to 12.5 ppm/° C. is well suited for use with an SOFC.
  • the sintered ceramic component having a CTE of 10.6 ppm/° C. to 12.5 ppm/° C. can be suitable for use with a gas-to-liquid membrane system.
  • the content may be expressed as an amount of MgO and another amount of Al 2 O 3 .
  • the MgO has a content that is at least 51 wt. %, at least 55 wt. %, or at least 60 wt. %, and in another embodiment, the MgO has a content that is no greater than 80 wt. %, no greater than 75 wt. %, or no greater than 70 wt. %. In a particular embodiment, the MgO has a content that is in a range of 51 wt. % to 80 wt. %, 55 wt. % to 75 wt. %, 60 wt. % to 70 wt. %.
  • the Al 2 O 3 has a content that is at least 20 wt. %, at least 25 wt. %, or at least 30 wt. %, and in another embodiment, the Al 2 O 3 has a content that is no greater than 49 wt. %, no greater than 45 wt. %, or no greater than 40 wt. %. In a particular embodiment, the Al 2 O 3 has a content that is in a range of 20 wt. % to 49 wt. %, 25 wt. % to 45 wt. %, 30 wt. % to 40 wt. %.
  • the desired dopants may help to achieve good density without having to sinter the ceramic component at too high of a temperature or having relatively high levels of undesired impurities.
  • the sintered ceramic component has a density that is at least 90% of theoretical density, at least 92% of theoretical density, or at least 94% of theoretical density, and in another embodiment, no greater than 99.9% of theoretical density, no greater than 99.5% of theoretical density, or no greater than 99.0% of theoretical density.
  • the sintered ceramic component has a density in a range of 90% to 99.9% of theoretical density, 92% to 99.5% of theoretical density, or 94% to 99% of theoretical density.
  • Density may also be expressed on a relative basis.
  • the relative densities can be expressed as a difference in percentages of theoretical density.
  • two different components have different compositions and are sintered under the same conditions.
  • One of the components may have a density that is 97% of theoretical density, and the other component may have a density that is 92% of theoretical density.
  • the density of the one component is 5% higher than the density of the other component.
  • the sintered ceramic component when sintered under the same conditions, has a density that is at least 3%, at least 6%, at least 9%, or at least 12% higher than a density of a different sintered ceramic component that includes at least 50 wt.
  • the sintered ceramic component when sintered under the same conditions, has a density that is no greater that 17%, no greater than 16%, no greater than 15%, or no greater than 14% higher than a density of a different sintered ceramic component that includes at least 50 wt. % MgO, all impurities are present at a combined impurity content of less than 0.7 wt.
  • the sintered ceramic component when sintered under the same conditions, has a density that is in a range of 3% to 17%, 6% to 16%, 9% to 15% higher than a density of a different sintered ceramic component that includes at least 50 wt. % MgO, all impurities are present at a combined impurity content of less than 0.7 wt. %, a remainder comprising Al 2 O 3 , and, other than MgO and Al 2 O 3 , other metal oxide is present at a content of at least 0.1 wt. %.
  • the color of the sintered ceramic component can be expressed in CIELAB coordinates.
  • the sintered ceramic component has L* is at least 65, at least 80, or at least 88; a* is in a range of ⁇ 1.0 to +7.0, ⁇ 0.3 to +2.0, or ⁇ 0.2 to +1.5; and b* is in a range of +4.0 to +20, +4.2 to +15, or +4.4 to +12.
  • a user of the sintered ceramic component may desire that the sintered ceramic component have a relatively white appearance.
  • the sintered ceramic component has L* is at least 85, at least 88, or at least 89; a* is in a range of ⁇ 1.0 to +1.0, ⁇ 0.3 to +0.7, or ⁇ 0.2 to +0.4; and b* is in a range of +4.0 to +9.0 +4.2 to +8.5, or +4.4 to +8.0. Contamination, rather than color, may more of a concern. Alternatively, a user may desire that the sintered ceramic component have a yellow or dark yellow appearance.
  • the sintered ceramic component has L* is at least 65, at least 70, or at least 75; a* is in a range of 0.0 to +7.0 +0.5 to +6.6 or +0.7 to +6.0; and b* is in a range of +5.0 to +20, +6.0 to +17, or +6.5 to +15.
  • a process of forming the sintered ceramic compound can include obtaining appropriate powders that make up the sintered ceramic compound.
  • Sources for the MgO and Al 2 O 3 may include those particular compounds or can include other sources.
  • powders of MgO and spinel MgAl 2 O 4
  • a powder including a fused MgO-containing MgAl 2 O 4 may be used.
  • the relative amounts of MgO and Al 2 O 3 may be controlled in a variety of ways.
  • One or more desired dopants can be added. Any of the dopants previously described may be added at the amounts previously described. In another embodiment, the dopants may be added using a different compound. For example, CaCO 3 may be used instead of or in conjunction with CaO.
  • CaCO 3 decomposes into CaO and CO 2 , thus, leaving CaO in the sintered ceramic component.
  • the amount of CaCO 3 in the starting material may be adjusted to account for a higher molecular weight as compared to CaO.
  • the powders may be agglomerated, milled, subjected to another particle size changing operation, or the like, if needed or desired. In an embodiment, the powders may have different particle sizes for the same material or different materials.
  • the powders for the ceramic component can be combined before, during or after the powders have an appropriate particle size.
  • the powders can include at least 50 wt.
  • each dopant of the at least one desired dopant has a desired dopant content of at least 0.1 wt. %; all impurities are present at a combined impurity content of less than 0.7 wt. %; and a remainder comprising Al 2 O 3 .
  • the process can further include combining the powders and a binder, another material, or a combination thereof to form a green mixture.
  • the binder or other material can include a polyacrylate, a polyvinyl alcohol, a polyethylene glycol, another suitable material to aid in mixing or binding the powders, or any combination thereof.
  • a solvent can be used if needed or desired.
  • the solvent can include water, alcohol, glycol, another suitable liquid that can aid in allow for better mixing of the powders and the binder, or any combination thereof.
  • One or more additional materials can be added if needed or desire. Such additional materials can include a surfactant, a polyvinyl alcohol, a polyvinyl butyral, a butyl benzyl phthalate, a fish oil, or any combination thereof.
  • the method can further include shaping the green mixture having a shape corresponding to the sintered ceramic component.
  • the shape can be larger than the final sintered ceramic component due to densification during a subsequent sintering operation.
  • the object can be heated during one or more operations to form the sintered ceramic component.
  • the object may be heated to a first temperature to drive out volatile components, such as the solvent.
  • the temperature can be in a range of 25° C. to 150° C. for a time in a range of 1 hour to 4 hours.
  • the pressure during volatile component drive off can be at atmospheric pressure or under vacuum pressure. If vacuum pressure is used, the pressure should not be so low as to cause any cracks, fractures, or other defects to form in the object.
  • the temperature can be increased to burn out the binder and any other carbon-containing material.
  • the temperature for the burn out operation can be in a range of 150° C. to 650° C. for a time in a range of 5 to 48 hours.
  • the pressure for the burn out can be performed at atmospheric pressure, at a higher pressure than atmospheric pressure, or under vacuum. Gas evolved during burn out may be difficult to remove if the pressure is too higher. In an embodiment, the pressure may not be greater than 30 kPa. If the pressure is too low, cracks, fractures, or other defects may form in the object. In an embodiment, the pressure may be at least 0.2 kPa-abs. In another embodiment, pressures higher or lower than recited may be used.
  • the burn out can be performed using an oxygen-containing gas, such as O 2 , ozone, N 2 O, NO, or the like. O 2 may be in the form of air (21 vol. % O 2 ) or may be provided at a concentration different from air. Air may be flown into the furnace during the burn out of the binder or other carbon-containing material.
  • the temperature can be further increased to form the sintered ceramic component.
  • the one or more dopants in the object can help to lower the sintering temperature of the material.
  • the sintering can be performed lower than the magnesia-alumina material by itself.
  • the sintering can be performed at a temperature less than 1600° C. Without dopant, the magnesia-alumina material will not properly sintered until the material is well above 1600° C., such as closer to 1800° C.
  • sintering is performed at a temperature of at least 1200° C., at least 1250° C., or at least 1300° C., and in another embodiment, sintering is performed at a temperature no greater than 1575° C., no greater than 1500° C., or no greater than 1450° C. In a particular embodiment, sintering is performed at a temperature in a range of 1200° C. to 1575° C., 1250° C. to 1550° C., or 1300° C. to 1450° C. The sintering may be performed for a time to allow sufficient sintering and densification to occur.
  • the time is at least 1 hour, at least 2 hours, or at least 3 hours, and in another embodiment, the time may be no greater than 50 hours, no greater than 20 hours, or no greater than 9 hours. In a particular embodiment, the time is in a range of 1 hour to 50 hours, 2 hours to 20 hours, or 3 hours to 9 hours.
  • Sintering can be performed at a pressure of at least atmospheric pressure (also referred to as pressureless sintering) to a relatively high pressure.
  • the pressure can be applied in the form of pressurized gas, hot pressing or hot isostatic pressing.
  • Sintering can be performed using an oxygen-containing gas, such as O 2 , ozone, N 2 O, NO, or the like.
  • O 2 may be in the form of air (21 vol. % O 2 ) or may be provided at a concentration different from air.
  • the operations described above may be performed during a single heating cycle or during different heating cycles. Additional operations may be performed during heating. For example, during cooling after sintering, the sintered ceramic component may be allowed to soak at a temperature to reduce the likelihood of building up too much strain within the component. Controlling the heating rate and cooling rate may also be used to reduce the likelihood of building up too much strain and cracking within the component.
  • the sintered ceramic component is well suited for use as a gas manifold or another component used in conjunction with a solid oxide fuel cell, a gas-to-liquid membrane system, or for another application where the sintered ceramic component configured such that it withstand exposure to a relatively high (i.e., greater than 400° C.) during normal operating conditions of an apparatus.
  • a sintered ceramic component having a final composition can include at least 50 wt. % MgO; at least one desired dopant, wherein each dopant of the at least one desired dopant has a desired dopant content of at least 0.1 wt. %; all impurities are present at a combined impurity content of less than 0.7 wt. %; and a remainder including Al 2 O 3 .
  • a process of forming a sintered ceramic component can include:
  • Embodiment 2 further including combining a first powder including MgO, a second powder including Al 2 O 3 , and a third powder including the at least one desired dopant before adding the binder.
  • Embodiment 2 further including combining a first powder including MgO and Al 2 O 3 and a second powder including the at least one desired dopant before adding the binder.
  • the sintered ceramic component or the process of Embodiment 14, wherein the CaO content is at least 0.2 wt. %, at least 0.3 wt. %, at least 0.4 wt. %, or at least 0.5 wt. %.
  • the sintered ceramic component of Embodiment 18, wherein the Y 2 O 3 content is at least 0.2 wt. %, at least 0.3 wt. %, at least 0.4 wt. %, or at least 0.5 wt. %.
  • MgO has a content that is at least 51 wt. %, at least 55 wt. %, or at least 60 wt. %.
  • MgO has a content that is no greater than 80 wt. %, no greater than 75 wt. %, or no greater than 70 wt. %.
  • MgO has a content that is in a range of 51 wt. % to 80 wt. %, 55 wt. % to 75 wt. %, 60 wt. % to 70 wt. %.
  • Al 2 O 3 has a content that is at least 20 wt. %, at least 25 wt. %, or at least 30 wt. %.
  • Al 2 O 3 has a content that is in a range of 20 wt. % to 49 wt. %, 25 wt. % to 45 wt. %, 30 wt. % to 40 wt. %.
  • An apparatus including the gas manifold of Embodiment 38, wherein the apparatus is a solid oxide fuel cell, and the gas manifold is fluidly coupled to an electrode of the solid oxide fuel cell.
  • L* is at least 65, at least 80, or at least 88;
  • a* is in a range of ⁇ 1.0 to +7.0, ⁇ 0.3 to +2.0, or ⁇ 0.2 to +1.5;
  • b* is in a range of +4.0 to +20, +4.2 to +15, or +4.4 to +12.
  • L* is at least 85, at least 88, or at least 89;
  • a* is in a range of ⁇ 1.0 to +1.0, ⁇ 0.3 to +0.7, or ⁇ 0.2 to +0.4;
  • b* is in a range of +4.0 to +9.0 +4.2 to +8.5, or +4.4 to +8.0.
  • L* is at least 65, at least 70, or at least 75;
  • a* is in a range of 0.0 to +7.0 +0.5 to +6.6 or +0.7 to +6.0;
  • b* is in a range of +5.0 to +20, +6.0 to +17, or +6.5 to +15.
  • the examples presented below demonstrate that sintered ceramic components having compositions as described above may be formed at sintering temperatures that are less than 1600° C. and achieve desired densities and visible appearances.
  • the sintered ceramic components may have different colors depending on the dopants and dopant concentrations selected. Samples were generated for analysis of sintering temperatures, densities when sintered at 1550° C. for 4 hours, and color information of the sintered materials.
  • Impure Samples were generated with different compositions.
  • One sample was made using conventional commercial-grade starting materials that were relatively high in impurities and is referred to as the Impure Sample.
  • Samples were made with starting materials that had relatively low impurity levels and are referred to the Pure 1 Sample and the Pure 2 Sample.
  • Tables 1 and 2 below include particle size distributions and the compositions of the Impure and Pure 1 and 2 Samples.
  • d 10 , d 50 , and d 90 represent the 10 th percentile, 50 th percentile, and the 90 th percentile of the Impure and Pure Samples.
  • Impure and Pure Samples MgO Al 2 O 3 CaO Y 2 O 3 TiO 2 ZrO 2 a SiO 2 Na 2 O Sample wt. % wt. % ppm ppm ppm ppm ppm ppm Impure 64.6 35.1 6100 160 124 1600 1100 600 Pure 1 65.2 34.6 645 ⁇ 5 10 150 120 140 Pure 2 66.4 35.0 765 20 60 2600 190 65 a —ZrO 2 reported is the combination of ZrO 2 and HfO 2
  • samples were heated to 1600° C. at a rate of 10° C./minute to obtain data for dilatometry curves. Other samples were heated to 1550° C. for 4 hours in air to obtain densification data.
  • FIGS. 1 to 8 Dilatometry curves were generated for the samples and are included in FIGS. 1 to 8 , which have % dL/dT as a function of temperature during the heating to 1600° C.
  • FIG. 1 includes a dilatometry curve of the Impure Sample.
  • FIGS. 2 and 3 include dilatometry curves of the Pure 1 and Pure 2 Samples.
  • FIGS. 4 to 8 include the dilatometry curves for selected doped and co-doped samples.
  • FIG. 9 includes a plot of densification, expressed as percentage of theoretical density as a function of doping concentration for particular dopants.
  • the material for the Impure Sample has typically has a densification in a range of 95.7% to 98.8%.
  • Table 7 includes the densification data.
  • Samples were checked for their visible appearance to the human eye. Samples were inspected after densification, and after annealing the densified samples were annealed at 800° C. for 72 hours in air. Table 8 includes the visual appearance information.
  • YI E313 [D65/10] is yellowness as measured using ASTM standard E313 using the version in effect as of the filing date of this specification. D65 is the standard illuminant, and 10 refers to the angle of insert light. Table 9 includes color space coordinate and yellowness information.
  • the Impure Sample has good sintering and densification properties; however, the Impure Sample has a high level of impurities due to commercial-grade starting materials being used.
  • the Pure 1 Sample has a white appearance, but the density is 83% when exposed to 1550° C. for 4 hours. In some applications, a densification of at least 95% may be needed or desired. Thus, sintering would need to be performed at a temperature greater than 1600° C. or the exposure at 1600° C. or lower would be long, both of which are undesired.
  • the Pure 1 and 2 Samples have very low levels of impurities and have a white appearance. As compared to Pure 1 Sample, the Pure 2 Sample has a significantly higher ZrO 2 content; however, even at such a ZrO 2 content, the Pure 2 Sample still does not have sufficiently good sintering and density properties.
  • the CaO-doped samples have a white appearance and good sintering characteristics. After sintering at 1550° C. for 4 hours in air, the density is over 95% of theoretical density at a CaO content of 0.13 wt. % and higher. Overall, the density is the highest in a range of 0.40 wt. % to 0.55 wt. % CaO content. Higher CaO can be used; however, the higher content levels increase manufacturing costs and does not further improve density.
  • the Y2O3 1 sample has a white appearance. As the Y 2 O 3 content increases the sample becomes more yellow. At 2 vol. % and higher, the Y 2 O 3 -doped samples have a dark yellow appearance that can change to yellow when exposed at 800° C. for 72 hours in air. The sintering characteristics are good, but not as good as the CaO-doped samples. Based on the data, the density increases until the Y 2 O 3 content reaches 1.40 wt. % and then decreases.
  • the TiO 2 -doped samples have a white appearance.
  • the sintering characteristics are good, and between the sintering characteristics of the CaO-doped samples and the Y 2 O 3 -doped samples. Based on the data, the density increases until the TiO 2 content reaches 0.9 wt. % and then decreases.
  • Y1.0-Ca0.5-co-doped samples have a white appearance and with a density of 95.1%, the same as CaO 0.5 singly doped samples both in density and in appearance while higher than Y 1.0 (1.0 Vol %.Y 2 O 3 ) singly doped samples (91.8%).
  • the Y2.2-Ca0.84 has a higher density (97.4%) than the density of Y or Ca samples, regardless of Y or Ca content in their corresponding singly doped samples, and the Y2.2-Ca0.84 co-doped samples have dark yellow appearance, the same as Y 2 O 3 doped samples with a Y 2 O 3 content of 2.78 wt % and higher.

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US20170190624A1 (en) 2017-07-06
WO2016077085A1 (en) 2016-05-19
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