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WO2002094727A1 - Verre de soudure en tant que materiau d'assemblage pour application sous haute temperature, production et utilisation - Google Patents

Verre de soudure en tant que materiau d'assemblage pour application sous haute temperature, production et utilisation Download PDF

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Publication number
WO2002094727A1
WO2002094727A1 PCT/DE2002/001549 DE0201549W WO02094727A1 WO 2002094727 A1 WO2002094727 A1 WO 2002094727A1 DE 0201549 W DE0201549 W DE 0201549W WO 02094727 A1 WO02094727 A1 WO 02094727A1
Authority
WO
WIPO (PCT)
Prior art keywords
glass solder
glass
mixture
content
bao
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/DE2002/001549
Other languages
German (de)
English (en)
Inventor
Tanja Schwickert
Pisit Geasee
Reinhard Conradt
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Forschungszentrum Juelich GmbH filed Critical Forschungszentrum Juelich GmbH
Publication of WO2002094727A1 publication Critical patent/WO2002094727A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/24—Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0271—Sealing or supporting means around electrodes, matrices or membranes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
    • H01M8/241—Grouping of fuel cells, e.g. stacking of fuel cells with solid or matrix-supported electrolytes
    • H01M8/2425—High-temperature cells with solid electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the invention relates to a glass solder as a joining material for high-temperature use, in particular in a high-temperature fuel cell, and to its production and use.
  • Glass solders have been used for many years to connect glass, ceramic and metal parts with and to one another. For use in a high-temperature fuel cell, glass solders have to meet special requirements due to the high temperatures prevailing there. Glass solders are required when joining individual fuel cells and also when joining individual cells to a so-called fuel cell stack.
  • the joints of the connected components mostly ceramics and / or metals, must be gas-tight and electrically insulating in the long term up to temperatures of 1000 ° C.
  • the thermal expansion coefficient of the glass solder used is matched as well as possible to that of the components to be connected.
  • the BAS (barium aluminum silicate) glass has proven to be a glass solder suitable in principle for this task. It has been found that the crystallization process, the crystal phases and their proportion and the resulting porosity are of crucial importance for the gas tightness of the glass solder. By adding MgO, the tendency to crystallize could be improved and the volume crystallization increased.
  • oxides are at least 5% by weight and a maximum of 15% by weight.
  • the glass ceramic has a coefficient of thermal expansion of more than 10 x 10 "6 per K.
  • Glass solders for the assembly of high-temperature fuel cells which are based on a mixture of BaO-CaO-Si0 2, are also known.
  • the object of the invention is to provide a further glass solder as a joining material for high-temperature use, which has a thermal expansion adapted to the materials to be joined in the temperature range above 800.degree. tion coefficient ⁇ of more than 11 x 10 "6 K " 1 .
  • the glass solder according to claim 1 is based on a mixture of BaO, CaO and Si0 2 with the addition of Al 2 0 3 .
  • This mixture is particularly suitable for use in a high-temperature fuel cell as the joining material for a gas-tight and temperature-resistant connection, for example between a ceramic and a metal.
  • the mixture allows the properties of the glass solder, such as e.g. B. the coefficient of thermal expansion to that of the materials to be joined. This can be used to regularly prevent thermal tensions between the materials, which usually occur during operation and when starting and shutting down a fuel cell.
  • the glass solders according to the invention can be described in their compositions with the aid of a ternary triangular diagram, the three corners of the diagram representing the pure components BaO, CaO and SiO 2 and the content of the fourth component Al 2 O 3 being kept constant.
  • An advantageous embodiment of the glass solder has a BaO content of 20 to a maximum of 80% by weight, in particular 45 to 55% by weight, in the ternary mixture of BaO-CaO-SiO 2 .
  • Further advantageous compositions of the ternary mixture BaO-CaO-SiO 2 see contents of CaO of> 0 to a maximum of 30% by weight, in particular 7 up to 15% by weight, and Si0 2 contents of 20 to a maximum of 65% by weight, in particular from 35 to 45% by weight.
  • the Al 2 0 3 content is advantageously not more than 10% by weight, based on the four-component mixture.
  • a further advantageous embodiment of the glass solder provides for the addition of oxides with elements, in particular of divalent and / or trivalent ions from groups VA to VIIA and IIB to VB, to the four-component mixture.
  • the advantageous effects such as an increase in the glass transition temperature, the softening temperature and in particular the coefficient of thermal expansion, can be achieved.
  • the flow properties and the crystallization properties can be regularly improved by adding further oxides.
  • Suitable oxides with divalent ions are: SrO, MnO, ZnO and PbO.
  • Suitable oxides with trivalent ions are: B 2 0 3 and La 2 0 3 .
  • higher-quality oxides, such as Ti0 2 or V 2 0 5 are also possible as additives. According to the invention, the content of added oxides is limited to a maximum of 20% by weight, based on the overall system.
  • the selected components are first mixed according to their desired composition in powder form (mixed powder) and exposed to an increase in temperature such that the particles melt completely. Typical temperature ranges are around 1300 to 1500 ° C. Then will the melted mixed powder (glass solder) cooled.
  • the glass solder can be obtained both as a shaped piece or, for example, as a solid block.
  • the solder is introduced between the components to be joined.
  • the solder can already be applied or arranged as a finished molding or as a paste with the glass solder ground from the block, for example.
  • the actual joining process in which the joining connection is made, and the glass solder crystallizes to form the glass ceramic.
  • the temperatures for the joining process are regularly in the range from 700 to 1000 ° C., in particular in the range from 800 to 900 ° C., that is to say significantly lower than when the mixed powder is melted.
  • the glass ceramic according to the invention is used advantageously in joining processes for producing gas-tight and electrically insulating connections between ceramics and / or metals, for example in a high-temperature fuel cell and in particular when assembling stacks from such fuel cells.
  • Figure 3 Location of the glass-ceramic solders in the three-substance system BaO-CaO-Si0 2
  • Figure 4 Section of the four-substance system BaO-CaO-Si0 2 with 5 wt .-% Al 2 0 3 with advantageous compositions
  • Table 2 advantageous compositions for the glass solders according to the invention.
  • FIG. 1 shows the thermal expansion coefficients ⁇ ec h for various glass solders and the stack components, in particular substrate and steel, as a function of the temperature.
  • An anode material comprising a cermet made of nickel and zirconium oxide was examined as the substrate.
  • the thermal expansion coefficient ⁇ tec h of the materials also increases.
  • the stack components have coefficients of thermal expansion in the range from 10 to 11 x 10 "6 per K, and reach values in the range from 13 to 14 x 10 " 6 per K at temperatures from 900 to 1000 ° C.
  • the glass solders should be advantageous have an adapted coefficient of thermal expansion.
  • the glass solders presented here achieve thermal expansion coefficients in the range from 11 to 12 x 10 "6 at temperatures of 900 to 100 ° C per K. Furthermore, in the temperature range in which the operation of a high-temperature fuel cell takes place (750 - 950 ° C), there should be no sudden change in the coefficient of thermal expansion.
  • FIG. 2 shows the thermal expansion coefficients for the glass solders listed in Table 2 as a function of the temperature. All of the compositions shown advantageously have a coefficient of thermal expansion of more than 11 ⁇ 10 ⁇ 6 per K at temperatures above 800 ° C.
  • FIG. 3 shows a triangular diagram for the compositions of the ternary mixture of BaO-CaO-SiO 2 with the representation of the area which is particularly advantageous for the glass solders according to the invention.
  • the advantageous compositions result from the ternary range shown in the triangular diagram with the addition of up to 10% by weight of A1 2 0 3 , based on the four-component mixture then present.
  • FIG. 4 shows a section of the phase diagram of the four-substance system BaO-CaO-Si0 2 with 5% by weight Al 2 0 3 .
  • the coefficients of thermal expansion of the constitutional phases in the corners have been taken from the literature. The entire glass formation area in this system was examined both with experimental (adhesion tests, gas tightness tests, heating microscope, dilatometer and X-ray diffraction) as well as with theoretical methods (calculation of the mineral phases to be expected in the physico-chemical equilibrium state). It was shown that only a certain section of the system provides suitable solders. The glasses in the CaO-Si0 2 corner (CS), for example, are not suitable because of their low coefficient of thermal expansion.
  • Table 2 also shows particularly advantageous compositions in% by weight for the glass solders according to the invention, in which further oxides are added to the four-component system.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Electrochemistry (AREA)
  • Ceramic Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Glass Compositions (AREA)

Abstract

L'invention concerne la production et l'utilisation de verres de soudure à base d'un mélange de BaO-CaO-SiO2 additionné de Al2O3, qui présentent un coefficient de dilatation thermique supérieur à 11 x 10<-6>K<-1>. Le coefficient de dilatation thermique élevé de ces verres de soudure, typiquement bien adapté à des composants à assembler (céramiques, métaux), permet une liaison d'étanchéité aux gaz et d'isolation électrique particulièrement avantageuse entre la céramique et/ou le métal sous haute température. Ces verres de soudure trouvent notamment leur application dans l'assemblage de piles à combustible de manière à former des empilages de piles à combustible.
PCT/DE2002/001549 2001-05-08 2002-04-27 Verre de soudure en tant que materiau d'assemblage pour application sous haute temperature, production et utilisation Ceased WO2002094727A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10122327.7 2001-05-08
DE10122327A DE10122327A1 (de) 2001-05-08 2001-05-08 Glaslot als Fügematerial für den Hochtemperatureinsatz sowie Herstellung und Verwendung

Publications (1)

Publication Number Publication Date
WO2002094727A1 true WO2002094727A1 (fr) 2002-11-28

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PCT/DE2002/001549 Ceased WO2002094727A1 (fr) 2001-05-08 2002-04-27 Verre de soudure en tant que materiau d'assemblage pour application sous haute temperature, production et utilisation

Country Status (2)

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DE (1) DE10122327A1 (fr)
WO (1) WO2002094727A1 (fr)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004063110A3 (fr) * 2003-01-03 2004-10-21 Battelle Memorial Institute Materiau vitroceramique et son procede de fabrication
US7015163B2 (en) * 2000-10-13 2006-03-21 Heraeus Quarzglas Gmbh & Co. Kg Glass member resistant to plasma corrosion
WO2009030336A1 (fr) * 2007-08-31 2009-03-12 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Circuiterie et procédé d'encapsulage de celle-ci
WO2009038627A1 (fr) * 2007-09-21 2009-03-26 Siemens Energy, Inc. Générateur à pile à combustible à oxyde solide comprenant un matériau d'étanchéité en verre
WO2010099634A1 (fr) * 2009-03-06 2010-09-10 Institute Of Metal Research, Chinese Academy Of Sciences Technique de scellement
EP2343115A4 (fr) * 2008-10-01 2013-04-17 Hitachi Shipbuilding Eng Co Membrane de séparation à base de zéolite, procédé de production correspondant et liant
DE102012207405B3 (de) * 2012-05-04 2013-08-14 Schott Ag Glaskeramisches Fügematerial und dessen Verwendung
JP2014231469A (ja) * 2013-05-28 2014-12-11 ショット アクチエンゲゼルシャフトＳｃｈｏｔｔ ＡＧ ガラス質の又は少なくとも部分的に結晶質の接合材料及びその使用
CN112194499A (zh) * 2020-10-22 2021-01-08 北京理工大学 一种用于低温快速焊接异质陶瓷的焊料
CN114212998A (zh) * 2021-12-15 2022-03-22 西安赛尔电子材料科技有限公司 一种用于超级电容器盖组封接玻璃的制备方法及封接工艺

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102004047539A1 (de) * 2004-09-30 2006-04-06 Elringklinger Ag Dichtungsanordnung für einen Brennstoffzellenstapel und Verfahren zum Herstellen eines Brennstoffzellenstapels
DE102005002435A1 (de) * 2005-01-19 2006-07-27 Forschungszentrum Jülich GmbH Herstellung einer Glaskeramik sowie dessen Verwendung als Fügematerial für den Hochtemperatureinsatz
AT505141B1 (de) * 2007-05-04 2009-02-15 Alpps Fuel Cell Systems Gmbh Verbindung von chemischen oder thermischen reaktoren
US8664134B2 (en) 2009-03-04 2014-03-04 Schott Ag Crystallizing glass solders and uses thereof
CN102341357B (zh) 2009-03-04 2014-12-31 肖特公开股份有限公司 结晶化玻璃焊料和其用途
DE102009011182B4 (de) * 2009-03-04 2017-03-23 Schott Ag Kristallisierendes Glaslot, Komposite und dessen Verwendung
DE102010035251B4 (de) 2010-02-15 2013-09-26 Schott Ag Hochtemperatur-Glaslot und dessen Verwendung
US9296644B2 (en) 2010-02-15 2016-03-29 Schott Ag High-temperature glass solder and its uses
DE102013009001A1 (de) 2013-05-24 2014-11-27 Friedrich-Schiller-Universität Jena Kristallisierende, cristobalitfreie und elektrisch gut isolierende Glaslote mit hohen thermischen Ausdehnungskoeffizienten zum Fügen von Metallen und/oder Keramiken
DE102013224111B4 (de) * 2013-11-26 2017-01-12 Schott Ag Natriumbeständiges Fügeglas und dessen Verwendung, Fügeverbindung, Energiespeichereinrichtung und/oder Energieerzeugungseinrichtung

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US3173779A (en) * 1959-12-16 1965-03-16 Gen Electric Sealing and coating glaze
US4060423A (en) * 1976-07-27 1977-11-29 General Electric Company High-temperature glass composition
US4349692A (en) * 1981-02-23 1982-09-14 Motorola, Inc. Glass hermetic seal
US4693987A (en) * 1986-09-08 1987-09-15 Corning Glass Works Molybdenum sealing glasses
US4737685A (en) * 1986-11-17 1988-04-12 General Electric Company Seal glass composition
DE19857057C1 (de) * 1998-12-10 2000-04-13 Fraunhofer Ges Forschung Verwendung von alkalifreien Glaskeramiken als Fügematerial für den Hochtemperatureinsatz
US6124224A (en) * 1998-09-02 2000-09-26 Ferro Corporation High temperature sealing glass

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EP0907215B1 (fr) * 1997-10-02 2002-01-02 Siemens Aktiengesellschaft Rendre étanche une pile à combustible fonctionnant à haute température ou un empilement de piles à combustible fonctionnant à haute température

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3173779A (en) * 1959-12-16 1965-03-16 Gen Electric Sealing and coating glaze
US4060423A (en) * 1976-07-27 1977-11-29 General Electric Company High-temperature glass composition
US4349692A (en) * 1981-02-23 1982-09-14 Motorola, Inc. Glass hermetic seal
US4693987A (en) * 1986-09-08 1987-09-15 Corning Glass Works Molybdenum sealing glasses
US4737685A (en) * 1986-11-17 1988-04-12 General Electric Company Seal glass composition
US6124224A (en) * 1998-09-02 2000-09-26 Ferro Corporation High temperature sealing glass
DE19857057C1 (de) * 1998-12-10 2000-04-13 Fraunhofer Ges Forschung Verwendung von alkalifreien Glaskeramiken als Fügematerial für den Hochtemperatureinsatz

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7015163B2 (en) * 2000-10-13 2006-03-21 Heraeus Quarzglas Gmbh & Co. Kg Glass member resistant to plasma corrosion
WO2004063110A3 (fr) * 2003-01-03 2004-10-21 Battelle Memorial Institute Materiau vitroceramique et son procede de fabrication
WO2009030336A1 (fr) * 2007-08-31 2009-03-12 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Circuiterie et procédé d'encapsulage de celle-ci
US8097381B2 (en) 2007-09-21 2012-01-17 Siemens Energy, Inc. Solid oxide fuel cell generator including a glass sealant
WO2009038627A1 (fr) * 2007-09-21 2009-03-26 Siemens Energy, Inc. Générateur à pile à combustible à oxyde solide comprenant un matériau d'étanchéité en verre
EP2343115A4 (fr) * 2008-10-01 2013-04-17 Hitachi Shipbuilding Eng Co Membrane de séparation à base de zéolite, procédé de production correspondant et liant
US9022226B2 (en) 2008-10-01 2015-05-05 Hitachi Zosen Corporation Zeolite separation membrane, method for producing the same, and bonding agent
WO2010099634A1 (fr) * 2009-03-06 2010-09-10 Institute Of Metal Research, Chinese Academy Of Sciences Technique de scellement
DE102012207405B3 (de) * 2012-05-04 2013-08-14 Schott Ag Glaskeramisches Fügematerial und dessen Verwendung
US8999869B2 (en) 2012-05-04 2015-04-07 Schott Ag Glass-ceramic joining material and use thereof
JP2014231469A (ja) * 2013-05-28 2014-12-11 ショット アクチエンゲゼルシャフトＳｃｈｏｔｔ ＡＧ ガラス質の又は少なくとも部分的に結晶質の接合材料及びその使用
US9206076B2 (en) 2013-05-28 2015-12-08 Schott Ag Vitreous or partially crystalline joining material and uses of same
CN112194499A (zh) * 2020-10-22 2021-01-08 北京理工大学 一种用于低温快速焊接异质陶瓷的焊料
CN112194499B (zh) * 2020-10-22 2022-01-07 北京理工大学 一种用于低温快速焊接异质陶瓷的焊料
CN114212998A (zh) * 2021-12-15 2022-03-22 西安赛尔电子材料科技有限公司 一种用于超级电容器盖组封接玻璃的制备方法及封接工艺

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