WO1998038138A1 - Composition ceramique, son procede de production et son utilisation - Google Patents
Composition ceramique, son procede de production et son utilisation Download PDFInfo
- Publication number
- WO1998038138A1 WO1998038138A1 PCT/DE1998/000524 DE9800524W WO9838138A1 WO 1998038138 A1 WO1998038138 A1 WO 1998038138A1 DE 9800524 W DE9800524 W DE 9800524W WO 9838138 A1 WO9838138 A1 WO 9838138A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- ceramic
- weight
- oxides
- composition according
- oxidic
- Prior art date
Links
- 239000000919 ceramic Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 9
- 239000000203 mixture Substances 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 239000011241 protective layer Substances 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 6
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 5
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 4
- 238000007650 screen-printing Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000002241 glass-ceramic Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000011575 calcium Substances 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011195 cermet Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000006112 glass ceramic composition Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002681 magnesium compounds Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007569 slipcasting Methods 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
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
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
-
- 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
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/403—Cells and electrode assemblies
- G01N27/406—Cells and probes with solid electrolytes
- G01N27/407—Cells and probes with solid electrolytes for investigating or analysing gases
- G01N27/4075—Composition or fabrication of the electrodes and coatings thereon, e.g. catalysts
Definitions
- the invention relates to a glass-like protective layer consisting of a ceramic composition, in particular for protecting mixed oxide electrodes of gas sensors, according to claim 1, and a method for their production.
- Ceramic, oxidic compositions have long been in use for the production of glass-ceramic layers and protective layers, in particular in the field of semiconductor technology, for protecting electronic components and for electrodes sensitive to temperature and chemical compounds, in particular electrodes of gas sensors.
- Protective layers used to date mostly consisting of aluminum oxide and similar oxides, which are applied using thick film printing technology or laminated on as green bodies, have the disadvantage that that this ceramic composition must be sintered at temperatures above 1500 ° C. These temperatures often damage underlying temperature-sensitive layers and components. It is also known to use glass-ceramic materials based on borosilicate glasses, which can be sintered at temperatures of less than 1000 ° in a reducing atmosphere.
- the ceramic, oxide composition based on the oxides of the elements Ca, Si, Ti and Al has the advantage that relatively low sintering temperatures are required during processing and that by using oxides, relatively chemically inert elements such as titanium and aluminum are chemically and temperature-stable protective layers can be produced.
- the oxidic composition according to the invention is advantageously mechanically extremely stable.
- this protective layer has very good adhesion to the substrate on which it is applied. Through the there is also no chemical stability with underlying layers, for example perovskites or doped mixed oxides etc.
- the ceramic, oxidic composition consists of 25 to 35% by weight of CaO, 35 to 40% by weight of SiO 2 , 8 to 12% by weight of TiO 2 and 15 to 25% by weight of Al 2 0 3 based on the total weight of the oxides.
- An extremely high mechanical and chemical stability of the ceramic oxide composition is achieved by this composition.
- portions of glassy carbon are added to the oxides, so that even porous, very hard and chemically stable, but at the same time gas-permeable layers and compositions are obtained in a simple manner.
- the oxides of the elements calcium, silicon, titanium and aluminum are mixed and melted together at a temperature of 1400 to 1800 ° C. and pulverized after cooling. Glassy carbon is then added to the powder mixture.
- the oxidic ceramic powder mixture obtained in this way is advantageously used as a screen printing paste, as a result of which glass-like protective layers can be made available for a large number of different substrates.
- the A screen printing paste according to the invention is applied to corresponding substrates, for example metallic or cermet conductor tracks or mixed oxide electrodes, in a simple manner by known processes.
- this oxidic ceramic composition is used as a gas-permeable protective layer for electrodes, in particular metal and mixed oxide electrodes of gas sensors, which have to have a particularly high temperature and chemical resistance.
- a ceramic, oxidic composition according to the invention consists of the following oxidic components:
- 20 g CaC0 3 (corresponds to 11.12 g CaO), 16.52 g Si0 2 , 4 g Ti0 2 and 7.64 g A1 2 0 3 are used and also melted in a platinum crucible at 1600 ° C .
- the cooled melt is broken out of the crucible and ground, for example, using a ball mill. It will 10% glass carbon added.
- the thus obtained - glass powder is placed in a so-called thick oil (Siebdruckpasten- base solution) "The thick oil consists for example of about 75% by weight of butyl carbitol (Diethylenglycolmonobutyl- ether), about 18% by weight of polyvinyl butyral, 7% by weight.
- the glass powder is mixed with the same weight of thick oil, printed on a sensor substrate and sintered. The sintering takes place at approx. 1150 ° C. and a very hard and porous layer is then obtained on, for example, a pre-fired mixed oxide electrode of a sensor. This also makes it possible to protect sensor materials that change or decompose at high processing temperatures of over 1200 ° C.
- the glass layer according to the invention thus obtained is harder than window glass and steel needles.
- the electrical conductivity is very low even at high temperatures. Adhesion to finished aluminum and zirconia substrates is very good.
- the mechanical and chemical resistance is given after long operation in corrosive burner gases.
- oxidic composition according to the invention is all common screen printing paste approaches and slip casting offsets.
- Next Sensor materials can also be protected from all oxidic materials that are exposed to large thermal and chemical stresses, for example resistance ceramics, etc.
- the protective layer according to the invention does not react with the sensor layer underneath.
- the catalytic activity towards the sample gas is low, so there is no falsified sensor signal.
- the protective layer has a low electrical conductivity, so that no electrical interference effects occur.
- there are no strongly diffusing ions in the glass composition according to the invention which would lead to poisoning of the sensor material.
- the oxidic ceramic composition according to the invention has a very high sulfate resistance, so that even engine exhaust gases do not react with the oxidic glass-ceramic protective layer.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Structural Engineering (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Molecular Biology (AREA)
- Electrochemistry (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Glass Compositions (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
L'invention concerne une composition céramique oxydique constituée des oxydes des éléments Ca, Si, Ti et Al, un procédé de production de cette composition, ainsi que l'utilisation de celle-ci pour former une couche protectrice vitreuse perméable aux gaz pour des électrodes, en particulier pour des électrodes à oxyde mixte de détecteurs de gaz.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19708105.3 | 1997-02-28 | ||
| DE1997108105 DE19708105C2 (de) | 1997-02-28 | 1997-02-28 | Keramische Zusammensetzung, Verfahren zu deren Herstellung sowie deren Verwendung |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO1998038138A1 true WO1998038138A1 (fr) | 1998-09-03 |
Family
ID=7821801
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/DE1998/000524 WO1998038138A1 (fr) | 1997-02-28 | 1998-02-21 | Composition ceramique, son procede de production et son utilisation |
Country Status (2)
| Country | Link |
|---|---|
| DE (1) | DE19708105C2 (fr) |
| WO (1) | WO1998038138A1 (fr) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6693053B2 (en) * | 2000-04-01 | 2004-02-17 | Robert Bosch Gmbh | Glass and glass powder mixture and use thereof for the production of a glass ceramic |
| US6699807B2 (en) * | 2000-04-01 | 2004-03-02 | Robert Bosch Gmbh | Glass ceramic material, method for producing the same and spark plug containing such a glass ceramic material |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006126056A (ja) * | 2004-10-29 | 2006-05-18 | Tdk Corp | 二酸化炭素センサ |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3151206A1 (de) * | 1980-12-27 | 1982-07-08 | Central Glass Co., Ltd., Ube, Yamaguchi | Glasiertes, keramisches traegermaterial |
| WO1995016646A1 (fr) * | 1993-12-18 | 1995-06-22 | Robert Bosch Gmbh | Procede de realisation d'une ou plusieurs cavites dans ou sous le revetement d'un substrat |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3743260C2 (de) * | 1987-12-19 | 1998-11-05 | Deutz Ag | Hubkolbenmaschine, insbesondere Brennkraftmaschine in Reihenbauart, die zumindest teilweise luftgekühlt ist |
| DE4004102C1 (en) * | 1989-02-17 | 1990-10-04 | Porzellanfabrik Friesland Bentz Gmbh & Co Kg, 2930 Varel, De | Ceramic material for mfg. refractory ware - comprises silicon di:oxide, aluminium oxide, iron (III) oxide, titanium di:oxide, magnesium oxide, calcium oxide, potassium oxide, etc. |
-
1997
- 1997-02-28 DE DE1997108105 patent/DE19708105C2/de not_active Expired - Fee Related
-
1998
- 1998-02-21 WO PCT/DE1998/000524 patent/WO1998038138A1/fr active Application Filing
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3151206A1 (de) * | 1980-12-27 | 1982-07-08 | Central Glass Co., Ltd., Ube, Yamaguchi | Glasiertes, keramisches traegermaterial |
| WO1995016646A1 (fr) * | 1993-12-18 | 1995-06-22 | Robert Bosch Gmbh | Procede de realisation d'une ou plusieurs cavites dans ou sous le revetement d'un substrat |
Non-Patent Citations (2)
| Title |
|---|
| M. A. VILLEGAS ET AL: "Propiedades y caracterizacion estructural de vidrios del sistema CaO-TiO2-Al2O3-SiO2", BOLETIN DE LA SOCIEDAD ESPANOLA DE CERAMICA Y VIDRIO., vol. 34, no. 3, 1995, MADRID ES, pages 135 - 139, XP002068948 * |
| SHCHEPOCHKINA YU A: "ENAMEL FOR CAST IRON", GLASS AND CERAMICS, vol. 52, no. 3/04, 1 March 1995 (1995-03-01), pages 104, XP000542839 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6693053B2 (en) * | 2000-04-01 | 2004-02-17 | Robert Bosch Gmbh | Glass and glass powder mixture and use thereof for the production of a glass ceramic |
| US6699807B2 (en) * | 2000-04-01 | 2004-03-02 | Robert Bosch Gmbh | Glass ceramic material, method for producing the same and spark plug containing such a glass ceramic material |
Also Published As
| Publication number | Publication date |
|---|---|
| DE19708105A1 (de) | 1998-09-03 |
| DE19708105C2 (de) | 2001-02-08 |
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