EP0653898B1 - Verfahren zum Herstellen von keramischen Heizelementen - Google Patents

Verfahren zum Herstellen von keramischen Heizelementen Download PDF

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Publication number
EP0653898B1
EP0653898B1 EP94117182A EP94117182A EP0653898B1 EP 0653898 B1 EP0653898 B1 EP 0653898B1 EP 94117182 A EP94117182 A EP 94117182A EP 94117182 A EP94117182 A EP 94117182A EP 0653898 B1 EP0653898 B1 EP 0653898B1
Authority
EP
European Patent Office
Prior art keywords
conductors
metallization
ceramic
heating
paste
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.)
Expired - Lifetime
Application number
EP94117182A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0653898A3 (de
EP0653898A2 (de
Inventor
Alfred Dr. Thimm
Heinz Groschwitz
Peter Besold
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.)
Ceramtec GmbH
Original Assignee
Ceramtec 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 Ceramtec GmbH filed Critical Ceramtec GmbH
Publication of EP0653898A2 publication Critical patent/EP0653898A2/de
Publication of EP0653898A3 publication Critical patent/EP0653898A3/de
Application granted granted Critical
Publication of EP0653898B1 publication Critical patent/EP0653898B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
    • H05B3/28—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material
    • H05B3/286—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material the insulating material being an organic material, e.g. plastic
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
    • H05B3/28—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material
    • H05B3/283—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor embedded in insulating material the insulating material being an inorganic material, e.g. ceramic

Definitions

  • the invention relates to a method for producing an electrical heating element, in the case of the metallic heating conductor between ceramic insulating layers are embedded, whereby as current leads and as current leads Contacting recesses in the ceramic insulating layers with electrical conductive mass are filled.
  • a ceramic heater is known, the one contains ceramic body and a heating element that is on the ceramic Body is formed.
  • This heating element consists of several areas.
  • the first area is a heat generating area.
  • Electrical line areas are used for power supply and power dissipation and connection areas connect the heat generating area with the electrical Line areas.
  • the heat generating area is made from a cermet formed which is a ceramic material and mainly from at least contains a metallic material consisting of a precious metal.
  • the electrical Pipe areas are formed from a metallic material that consists mainly of at least one base metal or one Cermet, which contains a ceramic material and the metallic material.
  • the materials of the Heat generation part and the connecting conductor also. Contains here too the material of the heat generating part as a main component is a precious metal.
  • the interconnector must be specially designed to be more specific Contact resistance is not higher than half the specific one Volume resistance of the heat development conductors.
  • the process for producing the invention Heating element is defined in claim 1, and that The heating element according to the invention is in claim 7 Are defined.
  • high temperature resistant metallization paste in thick film technology applied.
  • Layers are made using the screen printing process Layer thicknesses of up to 100 ⁇ m achieved.
  • the ceramic insulation layers with the applied metallization pastes are then preferably first dried.
  • the drying conditions depend on the used Screen printing oil, generally over a period of 5 to 30 minutes Temperatures in the range of 40 to 150 ° C is dried.
  • a metallization paste is used that at least 70 wt .-% metal powder consisting of tungsten or molybdenum or mixtures thereof, and not more than 35% by weight of one containing glass phase-forming ceramic powder or powder mixture Aluminum oxide, aluminum nitride, titanium nitride, titanium carbide or tungsten carbide and additionally contains 5 to 35% by weight of an organic pasting medium.
  • Organic pasting media are in particular oils such as mineral oil, vegetable Suitable oils or synthetic oils such as screen printing oil or recycling oil, it can but also fats, waxes, agents such as thixotropic agents, rosin or lecithin to achieve better filling levels, bentonites to improve the Strength of the unfired paste and / or organic solvents used become.
  • oils such as mineral oil, vegetable Suitable oils or synthetic oils such as screen printing oil or recycling oil
  • it can but also fats, waxes, agents such as thixotropic agents, rosin or lecithin to achieve better filling levels, bentonites to improve the Strength of the unfired paste and / or organic solvents used become.
  • unburned ceramic foils to enable electricity to be transported perpendicular to the Foil surface contacting recesses in the context of the present Invention also called "vias", punched or drilled.
  • the metallization paste is using a printing process such as screen printing, roller screen printing, Offset printing or pad printing on still unfired ceramic foils transferred, creating the desired pattern on the film surface becomes.
  • the fully filled vias have a diameter of 0.1 to 0.5 mm, preferably 0.3 mm.
  • the layer thickness of the metallization for the conductor tracks can be between 5 and 100 ⁇ m, preferably between 10 and 15 ⁇ m.
  • the width of the conductor track should be at least 0.25 mm in order to safely avoid a burnout, preferably about 0.5 mm.
  • the paste For processing the paste, it is recommended to use the paste to fill the vias to be used with a viscosity of 150 to 500 Pa • s for the flat Metallization printing, however, is advantageous, the paste by appropriate Add further small amounts of screen printing oil to a viscosity in the range from 50 to 90 Pa • s.
  • the metallization paste is matched to the shrinkage of the film so that during sintering, neither due to insufficient shrinkage of the Metallization compared to the shrinkage of the ceramic star cracks in the Ceramic, still due to excessive shrinkage of the metallization paste Voids or star cracks appear in the via.
  • the vote on the Shrinkage occurs through the composition and grain sizes of the powders.
  • the non-glass phase forming contained in the metallization paste Ceramic powder preferably has an average grain size of ⁇ 10 ⁇ m, particularly preferably ⁇ 2 ⁇ m. The grain sizes are determined with a Lasergranulometer® CILAS 850 measured by ALCATEL.
  • the overall resistance should be as constant as possible, which results from the surface resistance of the burned-in conductor track and the The area of the conductor track in the film layer level is obtained by multiplication. In In practice, total resistances of approximately 1 to 1000 ohms are used for such Miniature heating elements required. The distance between neighboring ones Conductors should be ⁇ 0.4 mm if possible to prevent them from burning out avoid. The overall arrangement of the conductor tracks should be chosen so that the loop has a heating temperature as uniform as possible over its extent having. Then the outer metallization parts of the Contact surfaces are nickel-plated without current. For this, a commercially available Metallization bath, for example, based on hypophosphite Reducing agents are used. If necessary, an additional copper and / or silver-containing solder layer can be applied.
  • an adhesive aid made of an organic mixture with a binder can be applied over the entire surface of the ceramic films.
  • Such adhesive aids are known from US Pat. No. 5,021,287 and contain organic resins such as polyvinyl butyral or acrylic resins in an organic solvent and possibly also plasticizers such as phthalic acid esters or polyethylene glycols.
  • the separation takes place, whereby at the same time the later form of the Heating element is generated.
  • the separation can, for example, by Cutting or punching is done.
  • the final size of the heating element is due to the sintering process Temperatures ⁇ 1600 ° C generated in a reducing, humid atmosphere.
  • the Furnace atmosphere preferably has a composition of about 75% Hydrogen and 25% nitrogen, the mixture being at a temperature of 55 ° C is saturated with water vapor.
  • heating elements which are produced by the method according to the invention, is a continuous operating temperature between 50 and, depending on Material composition, 1100 h at temperatures up to 1800 ° C possible.
  • the upper operating temperature limit is mainly from the chemical Composition of the ceramic insulating layers and their content of softening phases.
  • the ceramic Insulating layers materials such as aluminum oxide, aluminum nitride, zirconium oxide, Silicon dioxide or titanium nitride used.
  • the heating elements can be used as heating elements for Oxygen sensors or other measuring probes, especially for the Automotive technology, in laboratory measuring devices and infrared measuring transmitters or in the Heating technology, for example as an ignition element for igniting escaping flammable gases or as immersion heaters.
  • a 0.8 mm thick green film contained binder, plasticizer and Dispersant primarily aluminum oxide and 4% of a quartz-containing glass-forming offset.
  • the foil was cut with blades into cards that Recesses for the vias were made mechanically punched.
  • the vias were screen printed with a metallizing paste, which in addition to 84% by weight of tungsten with an average grain size of 2.5 ⁇ m 16% by weight of a fine-grained alumina with an average grain size of 1 ⁇ m and additionally 15% by weight as an organic pasting medium Screen printing oil, based on the weight of the solids content, contained.
  • Screen printing oil based on the weight of the solids content, contained.
  • For the Processing of the paste was a viscosity of 75 Pa • s for surface pressure and set to 175 Pa • s for the pressure of the vias.
  • FIG. 1 A graphical representation of this arrangement is illustrated in Figure 1.
  • the ceramic films 1 with the vias 2 can be recognized by reference numerals.
  • the Vias 2 are filled with via fillings, not shown.
  • the metallizations 4 are arranged in such a way that interconnect leads 5 and heating loops 6 result, the latter forming the heating area 7.
  • This stack of cards was pressed under a pressure of 90,000 hPa at a temperature of 90 ° C.
  • Several individual parts were cut from the laminate using a cutting tool.
  • the distance of the loop-shaped structure inside the heating element from the lateral outer edge of the heating element was 0.5 mm.
  • the rod-shaped heating elements were sintered under protective gas (moist mixture of nitrogen and hydrogen) at a temperature of 1630 ° C. in a hood furnace.
  • protective gas moist mixture of nitrogen and hydrogen
  • the ceramic material aluminum oxide with a content of 96% by weight Al 2 O 3 was produced, on the other hand, the conductor tracks were also sintered in a co-firing process.
  • the fully filled vias were 0.3 mm in diameter.
  • the layer thickness of the conductor track metallization was 12 ⁇ m and its width was 0.5 mm.
  • the surface resistance achieved with the conductor tracks according to Example 1 was 5 m ⁇ / cm 2 .
  • the finished heating element each had a width and height of approximately 2.5 mm and a length of its heating area of approximately 18 mm. The measurements made on the finished heating element are described after the examples and compared in a table.
  • Example 2 Analogously to Example 1, the same ceramic material was used made of 96% by weight aluminum oxide and 4% by weight quartz-containing, glass-forming Offset a heating element made with the same dimensions. One and only The difference was that the metallization paste consisted of 100% by weight Tungsten with an average particle size of 2.5 ⁇ m plus that for the Processing as a paste required the amount of screen printing oil. It's going on the measurement results referenced to the examples.
  • Ceramic film is analogous to the manufacturing process of Example 1.
  • ceramic material was an aluminum nitride with 3 wt .-% aluminum oxide and 4 wt% yttria.
  • a card was made from a unfired ceramic film with the help of those described below Metallizing paste printed with a wavy or meandering structure.
  • vias were mechanically created with a Stamped metal needle.
  • the metallization paste consisted of 84% by weight of molybdenum and 8% by weight Aluminum oxide and a further 8% by weight aluminum nitride.
  • the powders were fine Grain sizes as described in Example 1.
  • the metallizing paste was made with Screen printing oil adjusted to the viscosity described in Example 1.
  • the manufacturing process for a substantially annular heating element was in all points identical to the production processes of Examples 1 and 2.
  • Ceramic material was aluminum nitride with 10 wt .-% aluminum oxide and 3 wt .-% yttrium oxide.
  • the heatable Zone can be characterized by a slight shift in contact areas and vias the outer edge of the component become almost circular.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Surface Heating Bodies (AREA)
  • Resistance Heating (AREA)
  • Apparatuses And Processes For Manufacturing Resistors (AREA)
EP94117182A 1993-11-11 1994-10-31 Verfahren zum Herstellen von keramischen Heizelementen Expired - Lifetime EP0653898B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4338539A DE4338539A1 (de) 1993-11-11 1993-11-11 Verfahren zum Herstellen von keramischen Heizelementen
DE4338539 1993-11-11

Publications (3)

Publication Number Publication Date
EP0653898A2 EP0653898A2 (de) 1995-05-17
EP0653898A3 EP0653898A3 (de) 1996-01-17
EP0653898B1 true EP0653898B1 (de) 2003-05-14

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP94117182A Expired - Lifetime EP0653898B1 (de) 1993-11-11 1994-10-31 Verfahren zum Herstellen von keramischen Heizelementen

Country Status (4)

Country Link
US (1) US5560851A (ja)
EP (1) EP0653898B1 (ja)
JP (1) JP3664757B2 (ja)
DE (2) DE4338539A1 (ja)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2975951B1 (en) 2013-03-22 2018-12-05 British American Tobacco (Investments) Ltd Heating smokeable material

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KR101961290B1 (ko) * 2013-12-31 2019-03-25 한온시스템 주식회사 Ｐｔｃ 히터
CN104582024B (zh) * 2014-12-19 2016-07-06 苏州路路顺机电设备有限公司 一种分段冷却用加热管及其使用方法
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GB201720338D0 (en) 2017-12-06 2018-01-17 British American Tobacco Investments Ltd Component for an aerosol-generating apparatus
EP3775693A4 (en) 2018-03-27 2021-12-22 SCP Holdings, an Assumed Business Name of Nitride Igniters, LLC. HOT SURFACE IGNITION DEVICES FOR COOKING PLATES
TWI801559B (zh) * 2018-04-17 2023-05-11 美商瓦特洛威電子製造公司 鋁製加熱器
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DE102020200639A1 (de) * 2020-01-21 2021-07-22 Eberspächer Catem Gmbh & Co. Kg Elektrische Heizvorrichtung
CN113248237A (zh) * 2021-06-15 2021-08-13 江苏天宝陶瓷股份有限公司 一种远红外陶瓷加热器的制造方法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2975951B1 (en) 2013-03-22 2018-12-05 British American Tobacco (Investments) Ltd Heating smokeable material

Also Published As

Publication number Publication date
JPH07192906A (ja) 1995-07-28
EP0653898A3 (de) 1996-01-17
US5560851A (en) 1996-10-01
DE59410284D1 (de) 2003-06-18
EP0653898A2 (de) 1995-05-17
JP3664757B2 (ja) 2005-06-29
DE4338539A1 (de) 1995-05-18

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