IPC분류정보
국가/구분 |
United States(US) Patent
등록
|
국제특허분류(IPC7판) |
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출원번호 |
UP-0341533
(2006-01-30)
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등록번호 |
US-7838460
(2011-01-22)
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우선권정보 |
JP-2005-022155(2005-01-28) |
발명자
/ 주소 |
- Shimazu, Takashi
- Tsuji, Ryusuke
- Sobukawa, Hideo
- Seno, Yoshiki
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출원인 / 주소 |
- Kabushiki Kaisha Toyota Chuo Kenkyusho
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대리인 / 주소 |
Oblon, Spivak, McClelland, Maier & Neustadt, L.L.P.
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인용정보 |
피인용 횟수 :
0 인용 특허 :
2 |
초록
▼
A nanoporous metal oxide material comprising two or more metal oxides, wherein the nanoporous metal oxide material has ceria content of 10 to 60 weight %, zirconia content of 20 to 90 weight %, and alumina content of 70 weight % or less, and has nanopores whose diameters are 10 nm or less, and the m
A nanoporous metal oxide material comprising two or more metal oxides, wherein the nanoporous metal oxide material has ceria content of 10 to 60 weight %, zirconia content of 20 to 90 weight %, and alumina content of 70 weight % or less, and has nanopores whose diameters are 10 nm or less, and the metal oxides are homogeneously dispersed in a wall constituting the nanopores.
대표청구항
▼
What is claimed is: 1. A nanoporous metal oxide material comprising two or more metal oxides, wherein the nanoporous metal oxide material has a ceria content of 10 to 60 weight %, a zirconia content of 20 to 90 weight %, and an alumina content of 70 weight % or less, and has nanopores whose diamete
What is claimed is: 1. A nanoporous metal oxide material comprising two or more metal oxides, wherein the nanoporous metal oxide material has a ceria content of 10 to 60 weight %, a zirconia content of 20 to 90 weight %, and an alumina content of 70 weight % or less, and has nanopores whose diameters are 10 nm or less, and the metal oxides are homogeneously dispersed in a wall constituting the nanopores; and wherein when spectra for all metal elements of metal oxides whose content in the nanoporous metal oxide material is 10 at % or more are measured by energy dispersive X-ray spectroscopy at measuring points in a region where a sample thickness can be regarded as almost constant using transmission electron microscope with an electron beam diameter of 1.0 nm and an accelerating voltage of 200 kV, a mean Xm of relative intensity ratio X derived by converting integrated intensity of fluorescent X-ray peak of each metal element in obtained spectra to relative ratio, and a second moment ν2 around the mean Xm satisfy a condition expressed by a formula (I) for all the metal elements: ν2/Xm2≦0.02 (1) wherein Xm is the mean of relative intensity ratio X and is described by an equation Xm=(ΣX)/N (N being the number of measuring points), ν2 is the second moment around the mean Xm and is described by an equation ν2={Σ(X−Xm)2}/N, and ν2/Xm2 is a second moment normalized to the square of the mean Xm, in the formula (1). 2. The nanoporous metal oxide material according to claim 1, wherein the nanoporous metal oxide material is obtained by heat treating a fluid raw material composition comprising zirconia colloidal particles and/or a zirconium salt solution and ceria colloidal particles and/or a cerium salt solution without practical coprecipitation after mixing the composition at a shear rate of 10,000 sec−1 or higher. 3. The nanoporous metal oxide material according to claim 2, wherein the fluid raw material composition further comprises one or more of alumina colloidal particles and an aluminum salt solution. 4. The nanoporous metal oxide material according to claim 1, further comprising at least one powder selected from the group consisting of a zirconia powder, a ceria powder and an alumina powder, each of the powders having an average particle size of 0.01 to 50 μm. 5. The nanoporous metal oxide material according to claim 1, wherein when an equation (2) is obtained by an arbitrary line analysis of a range of 0.5 mm or more for all metal elements of metal oxides whose content is 10 at % or more in the nanoporous metal oxide material using X-ray microanalyzer with an electron beam diameter of 1.0 μm and an accelerating voltage of 15 kV, a K value expressed by the equation (2) satisfies a condition expressed by a formula (3) for all the metal elements in 65% or more of measuring points out of total measuring points: K value (%)=(X-ray intensity detected from nanoporous metal oxide material)/(X-ray intensity obtained from pure substance) (2) K - Km Km ≤ 0.02 ( 3 ) wherein K is the K value (%) at each measuring point and Km is a mean of K values of all the measuring points, in the formula (3). 6. The nanoporous metal oxide material according to claim 1, wherein when a surface height image of the nanoporous metal oxide material is measured arbitrarily with a tapping mode by a scanning probe microscope using a tip with a curvature radius of 5 nm with an interval of 3 nm or more and less than 4 nm, a height image H(L) derived as a function of a scan length L total of 2 μm or more satisfies a condition expressed by a formula (4) in 80% or more of measuring points out of total measuring points and also a second derivative H″ (L) derived from formulae (5) and (6) satisfies a condition expressed by a formula (7) in 60% or less of measuring points out of total measuring points: H(L)≦20 nm (4) wherein H(L) is a height image (nm) at each measuring point (scan length=L) in the formula (4); H ′ ( L ) = ⅆ H ⅆ L = H ( L + Δ L ) - H ( L ) Δ L H ″ ( L ) = ⅆ 2 H ⅆ L 2 = H ′ ( L + Δ L ) - H ′ ( L ) Δ L ( 5 ) ( 6 ) wherein H(L) is a height image (nm) at a measuring point where a scan length=L, H(L+ΔL) is a height image (nm) at a measuring point where a scan length=L+ΔL, ΔL is an interval (nm) among measuring points, H′(L) is a first derivative of a height image H(L), H′(L+ΔL) is a first derivative of a height image H(L+ΔL), and H″(L) is a second derivative of a height image H(L), in the formulae (5) and (6) and ΔL is set to 4 nm by linear interpolation among measuring points; and −0.05 nm−1≦H″(L)≦0.05 nm−1 (7). 7. The nanoporous metal oxide material according to claim 1, wherein when a measuring line is drawn arbitrarily for total of 400 μm or more on the nanoporous metal oxide material in an electron micrograph of a section of the nanoporous metal oxide material, a length ratio of a part where the measuring line intersects with a void portion formed in the nanoporous metal oxide material satisfies a condition that it is 10% or less of a total length of the measuring line. 8. The nanoporous metal oxide material according to claim 1, wherein when spectra for all metal elements of metal oxides whose content in the nanoporous metal oxide material is 10 at % or more are measured by energy dispersive X-ray spectroscopy at 10 or more arbitral measuring points using transmission electron microscope with an electron beam diameter of 1.0 nm and an accelerating voltage of 200 kV, a mean Xm of relative intensity ratio X derived by converting integrated intensity of fluorescent X-ray peak of each metal element in obtained spectra to relative ratio and a second moment ν2 around the mean Xm satisfy a condition expressed by a formula (8) for all the metal elements: ν2/Xm2≦0.1 (8) wherein Xm is the mean of relative intensity ratio X and is described by an equation Xm=(ΣX)/N (N being the number of measuring points), ν2 is the second moment around the mean Xm and is described by an equation ν2={Σ(X−Xm)2}/N, and ν2/Xm2 is a second moment normalized to the square of the mean Xm, in the formula (8). 9. The nanoporous metal oxide material according to claim 1, further comprising a noble metal supported on the surface of the nanoporous metal oxide material. 10. A catalyst support comprising: a substrate, and a coating comprising nanoporous metal oxide material formed from two or more metal oxides formed on the surface of the substrate, wherein the nanoporous metal oxide material has a ceria content of 10 to 60 weight %, a zirconia content of 20 to 90 weight %, and an alumina content of 70 weight % or less, and has nanopores whose diameters are 10 nm or less, and the metal oxides are homogeneously dispersed in a wall constituting the nanopores; and wherein when spectra for all metal elements of metal oxides whose content in the nanoporous metal oxide material is 10 at % or more are measured by energy dispersive X-ray spectroscopy at measuring points in a region where a sample thickness can be regarded as almost constant using transmission electron microscope with an electron beam diameter of 1.0 nm and an accelerating voltage of 200 kV, a mean Xm of relative intensity ratio X derived by converting integrated intensity of fluorescent X-ray peak of each metal element in obtained spectra to relative ratio and a second moment ν2 around the mean Xm satisfy a condition expressed by a formula (I) for all the metal elements: ν2/Xm2≦0.02 (1) wherein Xm is the mean of relative intensity ratio X and is described by an equation Xm=(ΣX)/N (N being the number of measuring points), ν2 is the second moment around the mean Xm and is described by an equation ν2={Σ(X−Xm)2}/N, and ν2/Xm2 is a second moment normalized to the square of the mean Xm, in the formula (1). 11. The catalyst support according to claim 10, wherein the nanoporous metal oxide material is obtained by heat treating the substrate after applied, without practical coprecipitation, with a fluid raw material composition comprising zirconia colloidal particles and/or a zirconium salt solution and ceria colloidal particles and/or a cerium salt solution mixed at a shear rate of 10,000 sec−1 or higher. 12. The catalyst support according to claim 11, wherein the fluid raw material composition further comprises one or more of alumina colloidal particles and an aluminum salt solution. 13. The catalyst support according to claim 10, further comprising at least one powder selected from the group consisting of a zirconia powder, a ceria powder and an alumina powder, each of the powders having an average particle size of 0.01 to 50 μm. 14. The catalyst support according to claim 10, wherein when an equation (2) is obtained by an arbitrary line analysis of a range of 0.5 mm or more for all metal elements of metal oxides whose content is 10 at % or more in the nanoporous metal oxide material using X-ray microanalyzer with an electron beam diameter of 1.0 μm and an accelerating voltage of 15 kV, a K value expressed by the equation (2) satisfies a condition expressed by a formula (3) for all the metal elements in 65% or more of measuring points out of total measuring points: K value (%)=(X-ray intensity detected from nanoporous metal oxide material)/(X-ray intensity obtained from pure substance) (2) K - Km Km ≤ 0.02 ( 3 ) wherein K is the K value (%) at each measuring point and Km is a mean of K values of all the measuring points, in the formula (3). 15. The catalyst support according to claim 10, wherein when a surface height image of the nanoporous metal oxide material is measured arbitrarily with a tapping mode by a scanning probe microscope using a tip with a curvature radius of 5 nm with an interval of 3 nm or more and less than 4 nm, a height image H(L) derived as a function of a scan length L total of 2 μm or more satisfies a condition expressed by a formula (4) in 80% or more of measuring points out of total measuring points and also a second derivative H″ (L) derived from formulae (5) and (6) satisfies a condition expressed by a formula (7) in 60% or less of measuring points out of total measuring points: H(L)≦20 nm (4) wherein H(L) is a height image (nm) at each measuring point (scan length=L) in the formula (4); H ′ ( L ) = ⅆ H ⅆ L = H ( L + Δ L ) - H ( L ) Δ L H ″ ( L ) = ⅆ 2 H ⅆ L 2 = H ′ ( L + Δ L ) - H ′ ( L ) Δ L ( 5 ) ( 6 ) wherein H(L) is a height image (nm) at a measuring point where a scan length=L, H(L+ΔL) is a height image (nm) at a measuring point where a scan length=L+ΔL, ΔL is an interval (nm) among measuring points, H′(L) is a first derivative of a height image H(L), H′(L+ΔL) is a first derivative of a height image H(L+ΔL), and H″(L) is a second derivative of a height image H(L), in the formulae (5) and (6) and ΔL is set to 4 nm by linear interpolation among measuring points; and −0.05 nm−1≦H″(L)≦0.05 nm−1 (7). 16. The catalyst support according to claim 10, wherein when a measuring line is drawn arbitrarily for total of 400 μm or more on the nanoporous metal oxide material in an electron micrograph of a section of the nanoporous metal oxide material, a length ratio of a part where the measuring line intersects with a void portion formed in the nanoporous metal oxide material satisfies a condition that it is 10% or less of a total length of the measuring line. 17. The catalyst support according to claim 10, wherein when spectra for all metal elements of metal oxides whose content in the nanoporous metal oxide material is 10 at % or more are measured with energy dispersive X-ray spectroscopy at 10 or more arbitral measuring points using transmission electron microscope with an electron beam diameter of 1.0 nm and an accelerating voltage of 200 kV, a mean Xm of relative intensity ratio X derived by converting integrated intensity of fluorescent X-ray peak of each metal element in obtained spectra to relative ratio and a second moment ν2 around the mean Xm satisfy a condition expressed by a formula (8) for all the metal elements: ν2/Xm2≦0.1 (8) wherein Xm is the mean of relative intensity ratio X and is described by an equation Xm=(ΣX)/N (N being the number of measuring points), ν2 is the second moment around the mean Xm and is described by an equation ν2={Σ(X−Xm)2}/N, and ν2/Xm2 is a second moment normalized to the square of the mean Xm, in the formula (8). 18. A catalyst for a hydrogen production reaction comprising the catalyst support according to claim 10 and a noble metal supported on the surface of the catalyst support.
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