Vitroceramic glass compositions for gaskets of apparatuses operating at high temperatures and assembling method using said compositions
원문보기
IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C03C-010/00
C03C-003/066
C03C-003/068
C03C-008/02
C03C-008/24
C03C-029/00
C04B-037/02
H01M-008/02
H01M-008/12
출원번호
US-0638561
(2011-03-31)
등록번호
US-9522842
(2016-12-20)
우선권정보
FR-10 52467 (2010-04-01)
국제출원번호
PCT/EP2011/055057
(2011-03-31)
§371/§102 date
20121219
(20121219)
국제공개번호
WO2011/121095
(2011-10-06)
발명자
/ 주소
Nonnet, Hélène
Connelly, Andrew
Khedim, Hichem
출원인 / 주소
Commissariat a l'énergie atomique et aux énergies alternatives
대리인 / 주소
Knobbe, Martens Olson & Bear LLP
인용정보
피인용 횟수 :
0인용 특허 :
12
초록▼
A vitroceramic glass composition consisting of SiO2, Al2O3, and CaO or of SiO2, Al2O3, CaO and SrO or of SiO2, Al2O3 and La2O3 is provided. In addition, a method and assembly of at least two parts using said composition is provided. Also, a gasket and assembly obtained by this method as well as a hi
A vitroceramic glass composition consisting of SiO2, Al2O3, and CaO or of SiO2, Al2O3, CaO and SrO or of SiO2, Al2O3 and La2O3 is provided. In addition, a method and assembly of at least two parts using said composition is provided. Also, a gasket and assembly obtained by this method as well as a high temperature electrolyzer (HTE) or solid oxide fuel cell (SOFC) comprising this gasket or this assembly are provided.
대표청구항▼
1. A vitroceramic glass composition, wherein the composition is selected from the group consisting of: a glass composition (A) consisting of in molar percentages: 36 to 43% of SiO2;9 to 13% of Al2O3;38 to 50% of CaO; and of one or several oxide(s) selected from the group consisting of the following
1. A vitroceramic glass composition, wherein the composition is selected from the group consisting of: a glass composition (A) consisting of in molar percentages: 36 to 43% of SiO2;9 to 13% of Al2O3;38 to 50% of CaO; and of one or several oxide(s) selected from the group consisting of the following oxides in the following molar percentages:4 to 5% of ZnO;2 to 9% of MnO2;2 to 6% of B2O3;0.1 to 1% of Cr2O3;0.1 to 4% of TiO2;a glass composition (B) comprising molar percentages of: 43 to 48% of SiO2;4 to 5% of Al2O3;8 to 10% of CaO;34 to 39% of SrO; and optionally of one or several oxide(s) selected from the group consisting of the following oxides in the following molar percentages:4 to 5% of ZnO;2 to 9% of MnO2;2 to 5% of B2O3;0.1 to 1% of Cr2O3; anda glass composition (C) comprising molar percentages of: 61 to 65% of SiO2;14 to 15% of Al2O3;18 to 20% of La2O3; and optionally of one or several oxide(s) selected from the following oxides in the following molar percentages:4 to 5% of ZnO;4 to 5% of MnO2;2 to 3% of B2O3;4 to 5% of CaO0.1 to 1% of Cr2O3; wherein the glass composition comprises more than 50% by weight of Crystalline phase, obtained by maintaining the glass composition at a temperature plateau from 600° C. to 1,000° C., for a duration of more than 1 hour said temperature plateau being reached by observing one or several temperature rise ramps at a rate from 0.5 to 3° C./minute. 2. The glass composition according to claim 1, which at the end of its elaboration and before any heat treatment only consists of an amorphous glassy phase. 3. The composition according to claim 1, wherein the composition (A) is selected from the group consisting of compositions A1 to A12 shown in the table below: Molar %Mass %SiO2Al2O3CaOZnOMnO2B2O3Cr2O3TiO2A1 (CAS)40.0038.6010.0016.3750.0045.03A2 (CAS_Cr2)39.8038.139.9516.1849.7544.490.51.21A3 (CAS_Cr)39.6037.689.9015.9849.5043.960.992.38A4 (CAS_B)39.0237.559.7615.9348.7843.802.442.72A5 (CAS_B2)38.1036.559.5215.5147.6242.644.765.29A6 (CAS_Mn2)39.0237.539.7615.9248.7843.782.442.77A7 (CAS_Mn)38.1036.529.5215.4947.6242.604.765.39A8 (CAS_Mn3)36.3634.659.0914.7045.4540.429.0910.23A9 (CAS_Mn_Cr)37.7435.699.4315.1447.1741.644.725.270.942.26A10 (CAS_Zn)38.1036.239.5215.3747.6242.274.766.14A11 (CAS2BT)41.4638.7111.7618.6239.4834.405.095.512.222.75A12 (CAS2B)42.439.8112.0219.1540.3735.385.205.66 4. The composition according to claim 1, wherein the composition (B) is selected from the group consisting of compositions B1 to B10 shown in the table below: SiO2Al2O3CaOSrOZnOMnO2B2O3Cr2O3Glass%%%%%%%%%%%%%%%%compositionmolmassmolmassmolmassmolmassmolmassmolmassmolmassmolmassB1 (SCAS)47.6236.554.766.209.526.8238.1050.43B2 (SCAS-Cr2)47.3936.214.746.159.486.7637.9149.960.470.92B3 (SCAS-Cr)47.1735.894.726.099.436.7037.7449.510.941.82B4 (SCAS-B)46.5135.794.656.079.306.6837.2149.382.332.07B5 (SCAS-B2)45.4535.064.555.959.096.9536.3648.384.554.06B6 (SCAS-Mn2)46.5135.784.656.079.36.6837.2149.362.332.11B7 (SCAS-Mn)45.4535.044.555.959.096.5436.3648.344.554.14B8 (SCAS-Mn3)43.4833.654.355.718.76.2834.7846.428.77.94B9 (SCAS-Mn—Cr)45.0534.434.55.849.016.4336.0447.504.54.060.91.74B10 (SCAS-Zn)45.4534.824.555.919.096.5036.3648.054.554.72 5. The composition according to claim 1, wherein the composition (C) is selected from the group consisting of compositions C1 to C7 shown in the table below: SiO2Al2O3La2O3ZnOMnO2B2O3CaOCr2O3Glass%%%%%%%%%%%%%%%%compositionmolmassmolmassmolmassmolmassmolmassmolmassmolmassmolmassC1 (LAS)65.0032.6815.0012.8020.0054.52C2 (LAS-Zn)61.9031.6014.2912.3819.0552.734.763.29C3 (LAS-Mn)61.9031.7414.2912.4319.0552.954.762.88C4 (LAS-B)63.4132.2114.6312.6119.5153.742.441.44C5 (LAS-Ca)61.9031.9314.2912.5019.0553.274.762.29C6 (LAS-Mn—Cr)61.3231.3514.1512.2818.8752.314.722.850.941.22C7 (LAS-Cr)64.3632.2714.8512.6419.8053.840.991.26 6. The glass composition according to claim 1, wherein the composition is in form of a powder. 7. A method for assembling at least two parts comprising the following successive steps: a) putting the parts into contact with a glass composition according to claim 1, thereby forming a first assembly comprising the parts and the glass composition;b) heating the assembly at a heating rate ranging between 0.5 and 3° C./min, said heating being optionally separated or interrupted by one or several temperature plateau(s), up to a temperature T1 sufficient for softening the glass composition in order to form a gasket between the parts; maintaining the assembly at a sufficient temperature T2, less than or equal to T1, and for a sufficient duration so that the glass composition solidifies and comprises more than 50% by weight of crystalline phase so as to form a second assembly comprising the parts and the gasket;c) cooling down the second assembly comprising the parts and the gasket to room temperature or an operating temperature. 8. The method according to claim 7, wherein the first assembly formed by the parts and the glass composition is maintained at a plateau at a temperature T2 from 600° C. to a 1,000° C. for a duration of more than 1 hour. 9. The method according to claim 7, wherein the step of putting the parts into contact with the glass composition comprises: forming a powder of the glass composition;suspending this powder in an organic binder so as to obtain a paste; andcoating at least one surface of the parts to be assembled with the obtained paste. 10. The method according to claim 9, wherein before reaching the temperature T1, a plateau is observed at a sufficient temperature T3 for a sufficient duration for removing the organic binder. 11. The method according to claim 10, wherein during step b), the following procedure is carried out: raising the temperature at 0.5° C./minute from room temperature, plateau at 400° C. for 120 minutes, raising the temperature at 3° C./minute from 400° C.; plateau at 800-950° C. for 50 hours to 120 hours, lowering the temperature at a rate of 3° C./minute down to room temperature or down to an operating temperature. 12. The method according to claim 7, wherein the step of putting the parts into contact with the glass composition comprises preparing a glass part having a shape of the gasket to be formed and then setting this part into place between surfaces of the parts to be assembled. 13. The method according to claim 12, wherein said glass part is prepared by compacting and then sintering a powder of the glass composition in a mold matching the shape of the glass part. 14. The method according to claim 12, wherein said glass part is a solid, massive glass block prepared by direct casting of the molten glass composition into a mold matching the shape of the glass part. 15. The method according to claim 7, wherein the parts to be assembled comprise a material selected from the group consisting of metals, metal alloys, ceramics, and composite materials comprising several of the aforementioned materials. 16. The method according to claim 15, wherein said at least two parts to be assembled comprise different materials. 17. The method according to claim 7, wherein said at least two parts to be assembled are parts of a high temperature electrolyzer > or of a high temperature fuel cell >. 18. A gasket obtained by the method according to claim 7. 19. An assembly obtained by the method according to claim 7. 20. A high temperature electrolyzer or high temperature fuel cell comprising a gasket according to claim 18. 21. A vitroceramic glass composition, wherein the composition is selected from the group consisting of: a glass composition (A) consisting of in molar percentages: 36 to 43% of SiO2;9 to 13% of Al2O3;38 to 50% of CaO; and of one or several oxide(s) selected from the group consisting of the following oxides in the following molar percentages:4 to 5% of ZnO;2 to 9% of MnO2;2 to 6% of B2O3;0.1 to 1% of Cr2O3,0.1 to 4% of TiO2;a glass composition (B) consisting of in molar percentages of: 43 to 48% of SiO2;4 to 5% of Al2O3;8 to 10% of CaO;34 to 39% of SrO; and optionally of one or several oxide(s) selected from the group consisting of the following oxides in the following molar percentages:4 to 5% of ZnO;2 to 9% of MnO2;2 to 5% of B2O3;0. 1 to 1% of Cr2O3; anda glass composition (C) consisting of in molar percentages of: 61 to 65% of SiO2;14 to 15% of Al2O3;18 to 20% of La2O3; and optionally of one or several oxide(s) selected from the following oxides in the following molar percentages:4 to 5% of ZnO;4 to 5% of MnO2;2 to 3% of B2O3;4 to 5% of CaO0.1 to 1% of Cr2O3,wherein the composition (A) is selected from the group consisting of compositions A1 to A12 shown in the table below: SiO2Al2O3CaOZnOMnO2B2O3Cr2O3TiO2MolarMassMolarMassMolarMassMolarMassMolarMassMolarMassMolarMassMolarMassGlass composition%%%%%%%%%%%%%%%%A1 (CAS)40.0038.6010.00 16.3750.0045.03A2 (CAS_Cr2)39.8038.139.9516.1849.7544.490.5 1.21A3 (CAS_Cr)39.6037.689.9015.9849.5043.960.992.38A4 (CAS_B)39.0237.559.7615.9348.7843.802.442.72A5 (CAS_B2)38.1036.559.5215.5147.6242.644.765.29A6 (CAS_Mn2)39.0237.539.7615.9248.7843.782.442.77A7 (CAS_Mn)38.1036.529.5215.4947.6242.604.765.39A8 (CAS_Mn3)36.3634.659.0914.7045.4540.429.0910.23 A9 (CAS_Mn_Cr)37.7435.699.4315.1447.1741.644.725.270.942.26A10 (CAS_Zn)38.1036.239.5215.3747.6242.274.766.14A11 (CAS2BT)41.4638.7111.76 18.6239.4834.405.095.512.222.75A12 (CAS2B)42.4 39.8112.02 19.1540.3735.385.205.66 22. The composition according to claim 21, which at the end of its elaboration and before any heat treatment only consists of an amorphous glassy phase. 23. The composition according to claim 21, wherein the glass composition comprises more than 50% by weight of crystalline phase, obtained by maintaining the glass composition according to claim 1 at a temperature plateau from 600° C. to 1,000° C., for a duration of more than 1 hour, said temperature plateau being reached by observing one or several temperature rise ramps at a rate from 0.5 to 3° C./minute. 24. The composition according to claim 21, wherein the composition (B) is selected from the group consisting of compositions B1 to B10 shown in the table below: SiO2Al2O3CaOSrOZnOMnO2B2O3Cr2O3%%%%%%%%%%%%%%%%Glass compositionmolmassmolMassMolMassmolmassmolmassmolmassmolmassmolmassB1 (SCAS)47.6236.554.766.209.526.8238.1050.43B2 (SCAS-Cr2)47.3936.214.746.159.486.7637.9149.960.470.92B3 (SCAS-Cr)47.1735.894.726.099.436.7037.7449.510.941.82B4 (SCAS-B)46.5135.794.656.079.306.6837.2149.382.332.07B5 (SCAS-B2)45.4535.064.555.959.096.9536.3648.384.554.06B6 (SCAS-Mn2)46.5135.784.656.079.3 6.6837.2149.362.332.11B7 (SCAS-Mn)45.4535.044.555.959.096.5436.3648.344.554.14B8 (SCAS-Mn3)43.4833.654.355.718.7 6.2834.7846.428.7 7.94B9 (SCAS-Mn—Cr)45.0534.434.5 5.849.016.4336.0447.504.5 4.060.9 1.74B10 (SCAS-Zn)45.4534.824.555.919.096.5036.3648.054.554.72 25. The composition according to claim 21, wherein the composition (C) is selected from the group consisting of compositions C1 to C7 shown in the table below: SiO2Al2O3La2O3ZnOMnO2B2O3CaOCr2O3Glass%%%%%%%%%%%%%%%%compositionmolmassmolmassmolmassmolmassmolmassmolmassmolmassmolmassC1(LAS)65.0032.6815.0012.8020.0054.52C2 (LAS-Zn)61.9031.6014.2912.3819.0552.734.763.29C3 (LAS-Mn)61.9031.7414.2912.4319.0552.954.762.88C4 (LAS-B)63.4132.2114.6312.6119.5153.742.441.44C5 (LAS-Ca)61.9031.9314.2912.5019.0553.274.762.29C6 (LAS-Mn—Cr)61.3231.3514.1512.2818.8752.314.722.850.941.22C7 (LAS-Cr)64.3632.2714.8512.6419.8053.840.991.26 26. The composition according to claim 21, wherein the composition is in form of a powder. 27. A method for assembling at least two parts comprising the following successive steps: a) putting the parts into contact with a glass composition according to claim 21, thereby forming a first assembly comprising the parts and the glass composition;b) heating the assembly at a heating rate ranging between 0.5 and 3° C./min, said heating being optionally separated or interrupted by one or several temperature plateau(s), up to a temperature T1 sufficient for softening the glass composition in order to form a gasket between the parts; maintaining the assembly at a sufficient temperature T2, less than or equal to T1, and for a sufficient duration so that the glass composition solidifies and comprises more than 50% by weight of crystalline phase so as to form a second assembly comprising the parts and the gasket;c) cooling down the second assembly comprising the parts and the gasket to room temperature or an operating temperature. 28. The method according to claim 27, wherein the first assembly formed by the parts and the glass composition is maintained at a plateau at a temperature T2 from 600° C. to a 1,000° C. for a duration of more than 1 hour. 29. The method according to claim 27, wherein the step of putting the parts into contact with the glass composition comprises: forming a powder of the glass composition;suspending this powder in an organic binder so as to obtain a paste; andcoating at least one surface of the parts to be assembled with the obtained paste. 30. The method according to claim 29, wherein before reaching the temperature T1, a plateau is observed at a sufficient temperature T3 for a sufficient duration for removing the organic binder. 31. The method according to claim 30, wherein during step b), the following procedure is carried out: raising the temperature at 0.5° C./minute from room temperature, plateau at 400° C. for 120 minutes, raising the temperature at 3° C./minute from 400° C.; plateau at 800-950° C. for 50 hours to 120 hours, lowering the temperature at a rate of 3° C./minute down to room temperature or down to an operating temperature. 32. The method according to claim 27, wherein the step of putting the parts into contact with the glass composition comprises preparing a glass part having a shape of the gasket to be formed and then setting this part into place between surfaces of the parts to be assembled. 33. The method according to claim 32, wherein said glass part is prepared by compacting and then sintering a powder of the glass composition in a mold matching the shape of the glass part. 34. The method according to claim 32, wherein said glass part is a solid, massive glass block prepared by direct casting of the molten glass composition into a mold matching the shape of the glass part. 35. The method according to claim 27, wherein the parts to be assembled comprise a material selected from the group consisting of metals, metal alloys, ceramics, and composite materials comprising several of the aforementioned materials. 36. The method according to claim 35, wherein said at least two parts to be assembled comprise different materials. 37. The method according to claim 27, wherein said at least two parts to be assembled are parts of a high temperature electrolyzer > or of a high temperature fuel cell >. 38. A gasket obtained by the method according to claim 27. 39. An assembly obtained by the method according to claim 27. 40. A high temperature electrolyzer or high temperature fuel cell comprising a gasket according to claim 38. 41. The method according to claim 9, wherein before reaching the temperature T1, a plateau is observed at a sufficient temperature T3 for a sufficient duration for removing the organic binder for a duration from 60 to 180 minutes. 42. The method according to claim 29, wherein before reaching the temperature T1, a plateau is observed at a sufficient temperature T3 for a sufficient duration for removing the organic binder for a duration from 60 to 180 minutes.
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이 특허에 인용된 특허 (12)
Bloom Ira D. (Bolingbrook IL) Ley Kevin L. (Bolingbrook IL), Compliant sealants for solid oxide fuel cells and other ceramics.
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