EP0653898A2 - Procédé de fabrication d'éléments chauffants céramiques - Google Patents

Procédé de fabrication d'éléments chauffants céramiques Download PDF

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Publication number
EP0653898A2
EP0653898A2 EP94117182A EP94117182A EP0653898A2 EP 0653898 A2 EP0653898 A2 EP 0653898A2 EP 94117182 A EP94117182 A EP 94117182A EP 94117182 A EP94117182 A EP 94117182A EP 0653898 A2 EP0653898 A2 EP 0653898A2
Authority
EP
European Patent Office
Prior art keywords
metallization
paste
ceramic
weight
heating element
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.)
Granted
Application number
EP94117182A
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German (de)
English (en)
Other versions
EP0653898B1 (fr
EP0653898A3 (fr
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/fr
Publication of EP0653898A3 publication Critical patent/EP0653898A3/fr
Application granted granted Critical
Publication of EP0653898B1 publication Critical patent/EP0653898B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • 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 which metallic heating conductors are embedded between ceramic insulating layers, contacting recesses in the ceramic insulating layers being filled with electrically conductive material as current leads and as current conductors.
  • Otsuka et al. describe in CERAMIC BULLETIN 60, pp. 540 ff (1981) that components made of ceramic materials, which mainly contain aluminum oxide or aluminum nitride, can be metallized with refractory metals such as tungsten or molybdenum, and that this metallization is then covered by a further layer of green ceramic and the composite can then be sintered to form the material.
  • Foil technology is particularly suitable for this.
  • an application as a heating element is possible in which large amounts of heat are preferably generated by the action of an electric current at those locations in the metallization pattern which have a high resistance.
  • the present invention was based on the object of specifying a manufacturing method for thin-walled ceramic heating elements, in which the structure is initially pre-formed with ceramic foils and with a high-temperature-resistant metallization, and in which a miniaturized high-performance heating element with permanent long-term stability can then be created by sintering the multilayer structure.
  • the heating conductors, the current leads and the current conductors are used as metallization paste containing 60 to 95% by weight of metal particles and 5 to 40% by weight of inorganic powder, based on the total solids content of the paste, are applied to the ceramic layers in the green state, that then the ceramic Layers with the applied metallization pastes are stacked on top of one another and then sintered.
  • the high-temperature-resistant metallization paste is applied using thick-film technology. Layers with layer thicknesses of up to 100 ⁇ m are achieved using the screen printing process. The ceramic insulating layers with the applied metallization pastes are then preferably first dried. The drying conditions depend on the screen printing oil used, with drying generally over a period of 5 to 30 minutes at temperatures in the range from 40 to 150 ° C.
  • a metallization paste is preferably used which contains at least 70% by weight of metal powder consisting of tungsten or molybdenum or mixtures thereof and at most 35% by weight of a non-glass-phase-forming ceramic powder or powder mixture containing aluminum oxide, aluminum nitride, titanium nitride, titanium carbide or tungsten carbide and in addition Contains 5 to 35 wt .-% of an organic pasting medium.
  • Oils such as mineral oil, vegetable oils or synthetic oils such as screen printing oil or recycling oil are particularly suitable as organic pasting media, but fats, waxes, adjusting agents such as thixotropic agents, rosin or lecithin can also be used to achieve better fill levels, bentonites to improve the strength of the unfired paste and / or organic solvents can be used.
  • contacting recesses also called “vias” in the context of the present invention
  • the metallizing paste is transferred to still unfired ceramic films using a printing process such as screen printing, roller screen printing, offset printing or pad printing, the desired pattern being produced 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 reliably avoid burning through, preferably about 0.5 mm.
  • the paste For the processing of the paste, it is recommended to use the paste to fill the vias with a viscosity of 150 to 500 Pa ⁇ s, for the flat metallization printing, however, it is advantageous to add a small amount of screen printing oil to the paste to a viscosity in the Range from 50 to 90 Pa ⁇ s.
  • the metallization paste is matched to the shrinkage of the film in such a way that during the sintering, there are no voids or star cracks in the via due to the metallization paste shrinking too little compared to the ceramic shrinkage, nor because of the metallization paste shrinkage too high.
  • the shrinkage is matched to the composition and grain size of the powder.
  • the non-glass-phase-forming ceramic powder contained in the metallization paste preferably has an average grain size of ⁇ 10 ⁇ m, particularly preferably ⁇ 2 ⁇ m. The grain sizes are measured with a laser granulometer ®CILAS 850 from ALCATEL.
  • a constant total resistance should be set, which is based on 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 practice, total resistances of approximately 1 to 1000 ohms are required with such miniature heating elements.
  • the distance between adjacent conductor tracks should be ⁇ 0.4 mm if possible to avoid burning out.
  • the overall arrangement of the conductor tracks should be selected so that the loop has a heating temperature that is as uniform as possible over its extent. Then the outer metallization parts of the contact surfaces can be nickel-plated.
  • a commercially available metallizing bath for example based on hypophosphite, can be used as a reducing agent for this purpose. If necessary, a copper and / or silver-containing solder layer can also 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 must now take place, the later shape of the heating element being produced at the same time.
  • the separation can take place, for example, by cutting or punching.
  • the final size of the heating element is generated by the sintering process at temperatures ⁇ 1600 ° C in a reducing, humid atmosphere.
  • the furnace atmosphere preferably has a composition of about 75% Hydrogen and 25% nitrogen, the mixture being saturated with water vapor at a temperature of 55 ° C.
  • the heating element is particularly miniaturized, special care must be taken with the temperature distribution and heat dissipation. In the heating area, care must be taken to ensure that the layer thickness of the conductor tracks is as uniform as possible in order to avoid local overheating in narrow spaces and places with a smaller layer thickness. In addition, poor coordination between the geometry and the thermal conductivity of the aluminum oxide material, the composition of the metallization and the conductor track design lead to burnout due to local overheating.
  • a continuous operating temperature between 50 and, depending on the material composition, 1100 h at temperatures up to 1800 ° C. can be achieved.
  • the upper operating temperature limit is primarily dependent on the chemical composition of the ceramic insulating layers and their content of softening phases. Materials such as aluminum oxide, aluminum nitride, zirconium oxide, silicon dioxide or titanium nitride are preferably used for the ceramic insulating layers.
  • the heating elements can be used as heating elements for oxygen sensors or other measuring probes, in particular for automotive technology, in laboratory measuring devices and infrared measuring transmitters or in heating technology, for example as an ignition element for igniting escaping flammable gases or as immersion heaters.
  • a 0.8 mm thick green film primarily contained aluminum oxide and 4% of a quartz-containing, glass-forming mixture.
  • the foil was cut into cards with blades, the recesses for the vias were 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, also 16% by weight of fine-grained alumina with an average grain size of 1 ⁇ m and an additional 15 as an organic pasting medium %
  • screen printing oil based on the weight of the solids content, contained.
  • a viscosity of 75 Pa ⁇ s for the surface pressure and 175 Pa ⁇ s for the pressure of the vias was set for the processing of the paste.
  • a loop-shaped structure was printed on the unfired and via-filled cards using the paste described using a screen printing machine using thick-film technology.
  • the printed cards were dried in air at 70 ° C.
  • a flat pattern was printed on other unfired cards, also with the described metallizing paste, using a screen printing machine. These metallization surfaces should be on the outside of the finished heating element and enable the electrical connection as contact surfaces. All printed cards were air dried at 70 ° C.
  • FIG. 1 A graphic representation of this arrangement is illustrated in FIG. 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.
  • the outer contact surfaces 8 can also be seen.
  • 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 between the loop-shaped structure inside the heating element and 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 wt .-% Al2O3 was generated, on the other hand, the conductor tracks were 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 ⁇ / cm2.
  • 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 are compared in a table.
  • Example 2 Analogously to Example 1, a heating element with the same dimensions was produced from the same ceramic material consisting of 96% by weight of aluminum oxide and 4% by weight of quartz-containing, glass-forming mixture. The only difference was that the metallizing paste consisted of 100 wt .-% tungsten with an average particle size of 2.5 microns plus the amount of screen printing oil necessary for processing as a paste. Reference is made to the measurement results following the examples.
  • the manufacturing process for a rod-shaped heating element, each with a contact surface at each of the rod ends and consisting of only two layers of ceramic film, is analogous to the manufacturing process of Example 1.
  • An aluminum nitride with 3% by weight aluminum oxide and 4% by weight was used as the ceramic material.
  • Yttrium oxide produced.
  • a card made of an unfired ceramic film was printed with the aid of the metallization paste described below with a wavy or meandering structure. Vias were mechanically punched into a second unfired ceramic card using a metal needle.
  • the metallization paste consisted of 84% by weight of molybdenum and 8% by weight of aluminum oxide and a further 8% by weight of aluminum nitride.
  • the powders had fine grain sizes as described in Example 1.
  • the metallization paste was adjusted to the viscosity described in Example 1 using screen printing oil.
  • the manufacturing process for an essentially annular heating element was identical in all points to the manufacturing processes of Examples 1 and 2.
  • Ceramic material aluminum nitride with 10 wt .-% aluminum oxide and 3 wt .-% yttrium oxide was used.
  • cards made of an unfired ceramic film were printed with the aid of the metallizing paste of Example 2 with an essentially ring-shaped and, if necessary, undulating or meandering structure.
  • the superimposed conductor tracks have different shapes or lengths, their electrical resistances and heating temperatures can be adjusted over the cross section of the conductor tracks.
  • the heatable zone can become almost circular due to a slight displacement of the contact surfaces and the vias on the outer edge of the component.

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  • 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 Procédé de fabrication d'éléments chauffants céramiques Expired - Lifetime EP0653898B1 (fr)

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 true EP0653898A2 (fr) 1995-05-17
EP0653898A3 EP0653898A3 (fr) 1996-01-17
EP0653898B1 EP0653898B1 (fr) 2003-05-14

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EP94117182A Expired - Lifetime EP0653898B1 (fr) 1993-11-11 1994-10-31 Procédé de fabrication d'éléments chauffants céramiques

Country Status (4)

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US (1) US5560851A (fr)
EP (1) EP0653898B1 (fr)
JP (1) JP3664757B2 (fr)
DE (2) DE4338539A1 (fr)

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WO2007130398A2 (fr) * 2006-05-03 2007-11-15 Watlow Electric Manufacturing Company Bornes d'alimentation pour dispositif chauffant en céramique et procédé de fabrication de ces bornes d'alimentation
CN104582024A (zh) * 2014-12-19 2015-04-29 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
EP2975951B1 (fr) * 2013-03-22 2018-12-05 British American Tobacco (Investments) Ltd Chauffage de matériau à fumer
US11318264B2 (en) 2017-01-13 2022-05-03 Nicoventures Trading Limited Aerosol generating device and article
US11589617B2 (en) 2017-01-05 2023-02-28 Nicoventures Trading Limited Aerosol generating device and article
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US7800020B2 (en) * 2007-01-19 2010-09-21 Ceva Carlos Jose Heating plate for hair straightening iron and its manufacturing process
US20080186045A1 (en) * 2007-02-01 2008-08-07 Matsushita Electric Industrial Co., Ltd. Test mark structure, substrate sheet laminate, multilayered circuit substrate, method for inspecting lamination matching precision of multilayered circuit substrate, and method for designing substrate sheet laminate
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007130398A2 (fr) * 2006-05-03 2007-11-15 Watlow Electric Manufacturing Company Bornes d'alimentation pour dispositif chauffant en céramique et procédé de fabrication de ces bornes d'alimentation
WO2007130398A3 (fr) * 2006-05-03 2008-03-20 Watlow Electric Mfg Bornes d'alimentation pour dispositif chauffant en céramique et procédé de fabrication de ces bornes d'alimentation
US7696455B2 (en) 2006-05-03 2010-04-13 Watlow Electric Manufacturing Company Power terminals for ceramic heater and method of making the same
US8242416B2 (en) 2006-05-03 2012-08-14 Watlow Electric Manufacturing Company Methods of making ceramic heaters with power terminals
EP2975951B1 (fr) * 2013-03-22 2018-12-05 British American Tobacco (Investments) Ltd Chauffage de matériau à fumer
EP3494815A1 (fr) * 2013-03-22 2019-06-12 British American Tobacco (Investments) Limited Chauffage de matériau fumable
CN104582024A (zh) * 2014-12-19 2015-04-29 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
US11589617B2 (en) 2017-01-05 2023-02-28 Nicoventures Trading Limited Aerosol generating device and article
US11318264B2 (en) 2017-01-13 2022-05-03 Nicoventures Trading Limited Aerosol generating device and article
US11623053B2 (en) 2017-12-06 2023-04-11 Nicoventures Trading Limited Component for an aerosol-generating apparatus

Also Published As

Publication number Publication date
DE4338539A1 (de) 1995-05-18
EP0653898B1 (fr) 2003-05-14
US5560851A (en) 1996-10-01
JPH07192906A (ja) 1995-07-28
DE59410284D1 (de) 2003-06-18
EP0653898A3 (fr) 1996-01-17
JP3664757B2 (ja) 2005-06-29

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