A method is described of producing a composite oxygen ion membrane and a composite oxygen ion membrane in which a porous fuel oxidation layer and a dense separation layer and optionally, a porous surface exchange layer are formed on a porous support from mixtures of (Ln1-xAx)wCr1-yByO3-δ and a doped
A method is described of producing a composite oxygen ion membrane and a composite oxygen ion membrane in which a porous fuel oxidation layer and a dense separation layer and optionally, a porous surface exchange layer are formed on a porous support from mixtures of (Ln1-xAx)wCr1-yByO3-δ and a doped zirconia. Preferred materials are (La0.8Sr0.2)0.95Cr0.7Fe0.3O3-δ for the porous fuel oxidation layer, (La0.8Sr0.2)0.95Cr0.5Fe0.5O3-δ for the dense separation layer, and (La0.8Sr0.2)0.95Cr0.3Fe0.7O3-δ for the porous surface exchange layer. Firing the said fuel activation and separation layers in nitrogen atmosphere unexpectedly allows the separation layer to sinter into a fully densified mass.
대표청구항▼
1. A method of producing an oxygen ion composite membrane comprising: forming a first layer on a porous support containing a first mixture of particles of (Ln1-xAx)wCr1-yByO3-δ and doped zirconia and pore formers, where Ln is La, Y, Pr, Ce or Sm, A is Ca or Sr, B is Fe, Mn, Co, Al, Ti or combination
1. A method of producing an oxygen ion composite membrane comprising: forming a first layer on a porous support containing a first mixture of particles of (Ln1-xAx)wCr1-yByO3-δ and doped zirconia and pore formers, where Ln is La, Y, Pr, Ce or Sm, A is Ca or Sr, B is Fe, Mn, Co, Al, Ti or combinations thereof, w is from about 0.9 to about 1.0, x is from about 0.1 to about 0.3 and y is from about 0.1 to about 0.6;the first mixture containing the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia such that when sintered, the first layer will contain the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia in a first volume percentage of (Ln1-xAx)wCr1-yByO3-δ of from about 30% to about 70% of the total solid mass;forming a second layer on the first layer that contains a second mixture of particles of (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia and that does not contain pore formers, where Ln is La, Y, Pr, Ce or Sm, A is Ca or Sr, B is Fe, Mn, Co, Al, Ti or combinations thereof, w is from about 0.9 to about 1.0, x is from about 0.1 to about 0.3 and y is from about 0.3 to about 0.7;the second mixture containing the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia such that when sintered, the second layer will contain the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia in a second volume percentage of (Ln1-xAx)wCr1-yByO3-δ of from about 30% to about 70% of the total solid mass;heating the first layer, the second layer and the porous support in nitrogen atmosphere so that said first layer partially sinters into a porous mass containing the first mixture of particles, thereby to provide a porous fuel oxidation layer and the second layer fully sinters into a densified mass containing the second mixture of particles, thereby to provide a dense separation layer. 2. The method of claim 1, wherein: a third layer is formed on the second layer containing a third mixture of particles of (Ln1-xCx)wCr1-yByO3-δ, the doped zirconia and pore formers, where Ln is La, Y, Pr, Ce or Sm, A is Ca or Sr, B is Fe, Mn, Co, Al, Ni or combinations thereof, w is from about 0.9 to about 1.0, x is from about 0.1 to about 0.3 and y is from about 0.4 to about 0.8;the third mixture having a third volume ratio of the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia such that when sintered, the third layer will contain the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia in a third volume percentage of (Ln1-xAx)wCr1-yByO3-δ of from about 30% to about 70% of the total solid mass; andthe third layer is heated so that said third layer partially sinters into a porous mass containing the third mixture of particles, thereby to provide a porous surface exchange layer. 3. The method of claim 2, wherein the doped zirconia is 10Sc1YSZ or 10Sc1CeSZ. 4. The method of claim 3, wherein: the (Ln1-xAx)wCr1-yByO3-δ within the first mixture of particles is (La1-xSrx)wCr1-yFeyO3-δ, where w is 0.95, x is 0.2 and y is 0.3; the (Ln1-xAx)wCr1-yByO3-δ within the second mixture of particles is (La1-xSrx)wCr1-yFeyO3-δ, where w is 0.95, x is 0.2 and y is 0.5; the (Ln1-xAx)wCr1-yByO3-δ within the third mixture of particles is (La1-xSrx)wCr1-yFeyO3-δ, where w is 0.95, x is 0.2 and y is 0.7; andthe porous support is formed from doped zirconium oxide or a mixture of MgO and MgAl2O4. 5. The method of claim 4, wherein the first volume percentage of (Ln1-xAx)wCr1-yByO3-δ is about 60% of the total solid mass, the second volume percentage of (Ln1-xAx)wCr1-yByO3-δ is about 50% of the total solid mass and the third volume percentage of (Ln1-xAx)wCr1-yByO3-δ is about 60% of the total solid mass. 6. The method of claim 5, wherein the porous support is of tubular or planar configuration. 7. The method of claim 6, wherein: the porous support is formed of 4YSZ and fired at a temperature of about 1050° C., so that it is not fully sintered prior to forming the first layer on the porous support;the first layer after having been formed on the porous support is dried at ambient temperature prior to coating the second layer on the first layer; andthe first layer, the second layer and the porous support are sintered at a temperature of about 1400° C. in nitrogen. 8. The method of claim 7, wherein the third layer is sintered at a temperature of from about 1250° C. to about 1350° C. in air. 9. The method of claim 6, wherein the first layer, the second layer and the third layer are sintered at a temperature of about 1400° C. in nitrogen, and wherein said first layer, second layer and/or said third layer are optionally formed by slurry coating. 10. The method of claim 2, wherein the first layer, the second layer and/or the third layer are formed by slurry coating. 11. The method of claim 10, wherein the doped zirconia is 10Sc1YSZ or 10Sc1CeSZ. 12. The method of claim 11, wherein the porous support is 4YSZ. 13. An oxygen ion composite membrane comprising: first and second layers on a porous support providing a porous fuel oxidation layer and a dense separation layer, respectively, for the oxygen ion composite membrane;each of the first and second layers containing a mixture of (Ln1-xAx)wCr1-yByO3-δ and doped zirconia, where for the first of the layers, Ln is La, Y, Pr, Ce or Sm, A is Ca or Sr, B is Fe, Mn, Co, Al, Ti or combinations thereof, w is 0.9-1.0, x is 0.1-0.3 and y is 0.1-0.6 and for the second of the layers, Ln is La, Y, Pr, Ce or Sm, A is Ca or Sr, and B is Fe, Mn, Co, Al or combinations thereof, w is 0.9-1.0, x is 0.1-0.3 and y is 0.3-0.7;the first of the layers containing the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia in a first volume percentage of (Ln1-xAx)wCr1-yByO3-δ of from about 30% to about 70% of the total solid mass; and the second of the layers containing the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia in a second volume percentage of (Ln1-xAx)wCr1-yByO3-δ of from about 30% to about 70% of the total solid mass. 14. The oxygen ion composite membrane of claim 13, wherein: a third layer is situated on the second layer to form a porous surface exchange layer and that also contains the mixture of (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia, where Ln is La, Y, Pr, Ce or Sm, A is Ca or Sr, B is Fe, Mn, Co, Al, Ni or combinations thereof, w is from about 0.9 to about 1.0, x is from about 0.1 to about 0.3 and y is from about 0.4 to about 0.8; andthe third layer containing the (Ln1-xAx)wCr1-yByO3-δ and the doped zirconia in a third volume percentage of (Ln1-xAx)wCr1-yByO3-δ of from about 30% to about 70% of the total solid mass. 15. The oxygen ion composite membrane of claim 14, wherein the doped zirconia is 10Sc1YSZ or 10Sc1CeSZ. 16. The oxygen ion composite membrane of claim 15, wherein: the (Ln1-xAx)wCr1-yByO3-δ within the first layer is (La1-xSrx)wCr1-yFeyO3-δ, where w is 0.95, x is 0.2 and y is 0.3;the (Ln1-xAx)wCr1-yByO3-δ within the second layer is (La1-xSrx)wCr1-yFeyO3-δ, where w is 0.95, x is 0.2 and y is 0.5;the (Ln1-xAx)wCr1-yByO3-δ within the third layer is (La1-xSrx)wCr1-yFeyO3-δ, where w is 0.95, x is 0.2 and y is 0.7; andthe porous support is formed from stabilized zirconia oxide or a mixture of MgO and MgAl2O4. 17. The oxygen ion composite membrane of claim 13 or claim 16, wherein the first volume percentage of (Ln1-xAx)wCr1-yByO3-δ is about 60% of the total solid mass, the second volume percentage of (Ln1-xAx)wCr1-yByO3-δ is about 50% of the total solid mass and the third volume percentage of (Ln1-xAx)wCr1-yByO3-δ is about 60% of the total solid mass. 18. The oxygen ion composite membrane of claim 16, wherein the porous support is of tubular or planar configuration. 19. The oxygen composite membrane of claim 17, wherein the porous support is formed from 4YSZ.
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