WO2006111445A1 - Resistance ceramique et procede de fabrication - Google Patents

Resistance ceramique et procede de fabrication Download PDF

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Publication number
WO2006111445A1
WO2006111445A1 PCT/EP2006/060896 EP2006060896W WO2006111445A1 WO 2006111445 A1 WO2006111445 A1 WO 2006111445A1 EP 2006060896 W EP2006060896 W EP 2006060896W WO 2006111445 A1 WO2006111445 A1 WO 2006111445A1
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WO
WIPO (PCT)
Prior art keywords
ceramic
green body
resistor
carbon fibers
carbon
Prior art date
Application number
PCT/EP2006/060896
Other languages
German (de)
English (en)
Inventor
Alexander Klonczynski
Martin Koehne
Original Assignee
Robert Bosch Gmbh
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Publication date
Application filed by Robert Bosch Gmbh filed Critical Robert Bosch Gmbh
Priority to JP2008507035A priority Critical patent/JP2008538541A/ja
Publication of WO2006111445A1 publication Critical patent/WO2006111445A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
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Definitions

  • the invention relates to a ceramic resistor and a method for its production and to a ceramic heater containing it after the
  • a ceramic resistor which is produced from an organosilicon polymer with the addition of a filler and whose electrical conductivity can be adjusted by adding a corresponding amount of molybdenum disilicide.
  • the filled polymer is cured at 200 0 C and then pyrolyzed at temperatures between 800 and 1400 0 C.
  • the resulting ceramic resistor is resistant to high temperatures; its long-term stability is limited, since molybdenum disilicide at higher temperatures of 400 to 800 0 C tends to oxidation and the resulting molybdenum oxides lead to a structural breakdown (so-called Molybdändisilicid plague).
  • the object of the present invention is to provide a ceramic resistor which, even in the context of applications at higher temperatures, exhibits a constant and sufficient electrical conductivity over long periods of time.
  • the ceramic resistor with the characterizing features of claim 1 solves the problem underlying the invention in an advantageous manner. It is particularly advantageous that the ceramic resistor has a largely freely selectable electrical conductivity, which is constant even in long-term operation, since it is not based on the addition of molybdenum disilide to the ceramic.
  • the ceramic resistor contains carbon fibers. The addition of carbon fibers causes an improvement in the electrical or thermal conductivity of the ceramic. Furthermore, their strength and impact resistance can be improved.
  • the carbon fibers used represent a cost-effective alternative to the substances previously used as electrically conductive fillers, such as metal silicides.
  • the ceramic resistor is present as an intermediate in its production
  • Green body which in turn contains carbon fibers or carbon fiber precursors.
  • carbon fiber precursors when using carbon fiber precursors, a cost-effective representation of the ceramic resistance is possible in an advantageous manner, since these are often generally available substances.
  • Characteristics of the ceramic resistance can be decisively influenced.
  • parallel aligned carbon fibers within the ceramic matrix lead to an anisotropic electrical conductivity of the ceramic resistor. If carbon fibers are used in the form of a fabric, in particular the strength or impact resistance of the ceramic improves. Furthermore, it is advantageous if the proportion of carbon fibers in the ceramic material of the ceramic resistor does not exceed a proportion of 40 vol.%, Since otherwise a shaping of the ceramic material by means of plastic-technical methods is no longer possible.
  • Carbon fibers coated with boron nitride In this way, the connection of the carbon fibers to the surrounding ceramic matrix can be suitably adjusted. Excessive bonding of the carbon fibers to the ceramic possibly leads to an increased risk of breakage.
  • Green bodies are preferably used polymer fibers. These are in particular polymers based on hydrocarbons. Also suitable are polyamides, polyesters, polyvinyl alcohols, polyimides, polyetherimides, PEEK, epoxy resins, amine resins, polyurethanes, polyamide-imides, cellulose or derivatives thereof and mixtures thereof.
  • the green body, from which the ceramic resistor can be produced is made on the basis of an organosilicon polymer.
  • the green body can be converted by pyrolysis at relatively moderate temperatures in a corresponding ceramic.
  • the green body at least one powder of a
  • the ceramic resistor according to the invention is formed of a ceramic material comprising carbon fibers. Furthermore, fillers for modifying the mechanical and electrical properties of the resistance material may be provided as constituents in addition to conventional excipients.
  • the carbon fibers may be in the form of long or short fibers or tissues as well as
  • Fiber bundles are used. Existence in the ceramic of dispersed carbon fibers leads - A -
  • an electrical heater can be produced on the basis of an electrically insulating ceramic.
  • the ceramic material itself can by thermolysis element organic polymer
  • Precursor compounds can be obtained. Such ceramics are referred to as so-called precursor ceramics. Alternatively, the ceramic material may be formed as a classic sintered ceramic.
  • Examples of possible fillers are molybdenum disilicide, silicon nitride,
  • Silicon powder titanium silicide, cerium oxide, bismuth oxide, barium oxide, silicon carbide, boron carbide, boron nitride, graphite and / or alumina in question.
  • the ceramic resistor is produced by heat treatment of a corresponding green body. Is the ceramic resistance based on a
  • the corresponding green body comprises as a ceramic precursor, for example, a polysiloxane, polysilsesquioxane, polysilazane, polyborosilazane, polysilane, polycarbosilane, an aluminoxane, a metal powder-filled aminoplast or mixtures thereof.
  • a ceramic precursor for example, a polysiloxane, polysilsesquioxane, polysilazane, polyborosilazane, polysilane, polycarbosilane, an aluminoxane, a metal powder-filled aminoplast or mixtures thereof.
  • An aluminoxane is understood to mean a polysiloxane in which at least partially silicon atoms are replaced by aluminum atoms.
  • Integration of carbon fibers into the precursor ceramic to be produced can be carried out by adding carbon fibers directly to the ceramic precursor or, alternatively, precursor compounds in the form of carbon fiber precursors or in the form of carbon fiber precursor-containing materials which form carbon fibers during the subsequent heat treatment.
  • polymer fibers are suitable as carbon fiber precursor. These are in particular fibers of polymers based on hydrocarbons such as polypropylene, polystyrene or polyethylene, fibers based on a polyamide such as aramid, a polyester, a polyvinyl alcohol, a polyimide, a polyetherimide, a polyetheretherketone (PEEK), an epoxy resin, an amine resin such as a melamine resin or urea resin, a polyurethane, a polyamide-imide, a phenolic resin, a polyacrylonitrile, a pitch, in particular a mesophase pitch, or based on cellulose or its derivatives such as acetylcellulose, viscose, Modal, cupro or acetate / triacetate (acetate rayon).
  • a polyacrylonitrile is advantageous.
  • the mentioned carbon fiber precursors can be added to the ceramic green body and, during the subsequent heat treatment of the ceramic base body, convert into corresponding carbon fibers. Another possibility is to first subject the said carbon fiber precursors or corresponding carbon fiber precursor containing materials to conversion to carbon fibers and then adding them to the ceramic green body. Exemplary representations of carbon fibers from corresponding carbon fiber precursor are tabulated below.
  • the incorporation of the carbon fiber precursors or carbon fibers into the green body can take place in the form of an additive, which is mixed in with the other constituents in the course of the production process.
  • Another possibility is to carry out the material of the ceramic resistor based on a sintered ceramic.
  • a ceramic slurry is formed from a ceramic powder which can be converted into a corresponding ceramic by means of a subsequent sintering process, from which a corresponding green body is produced.
  • Such ceramics can, for example, on the basis of
  • Silicon carbide alumina, mullite, silicon nitride, boron carbide, boron nitride, aluminum nitride or silicon-aluminum oxynitride (SiAlON).
  • the preparation of the nanopowder is advantageously carried out by electrical wire explosion.
  • nanopowders When using nanopowders is already at relatively low temperatures a high
  • the amount of added metal powder depends on the desired degree of attachment to the ceramic matrix. For a high fracture toughness of the ceramic composite is too strong or too weak connection of the carbon fibers to the
  • Too weak a connection shows up in the absence of a reinforcing effect of the fibers. Although a too strong connection increases the strength of the ceramic material, but does not prevent a so-called catastrophic fracture of the same.
  • Optimal is a connection of the carbon fibers to the ceramic portion of the
  • the pull-out force of the fiber in which it is mechanically detached from the ceramic matrix, is smaller than the strength of the matrix.
  • the pull-out force should be so high that a crack, if it is around a Fiber spread around and this is torn out of the ceramic matrix, by the tearing loses so much energy that the crack progress is slowed down or stopped at best.
  • the fracture toughness can be significantly increased.
  • a better connection of the carbon fibers to the precursor ceramic or sintered ceramic with a suitable choice of the additive can also be effected by bridge formation.
  • the particles of the additive come into contact with the precursor ceramic or sintered ceramic on one side and with the carbon fibers on the other side.
  • Semi-metals, metals, metal alloys and intermetallic compounds can be used as the additive, such as, for example, aluminum, boron, silicon, zirconium, molybdenum disilicide or tantalum disilicide.
  • the pull-out force can be increased by adding metal powders or additives, as already mentioned. However, it can also be lowered if this corresponds to the requirement profile. A reduction in the pull-out force, for example, by complete or partial coating of the carbon fiber precursor or the
  • Carbon fibers can be achieved with an inert, thermally stable release agent such as boron nitride, silicon nitride, silicon carbide, silicon carbonitride, boron carbonitride or silicon-boron-carbonitride. This avoids a strong bond between ceramic matrix and carbon fibers.
  • an inert, thermally stable release agent such as boron nitride, silicon nitride, silicon carbide, silicon carbonitride, boron carbonitride or silicon-boron-carbonitride.
  • the strength of the bond between the carbon fibers can be adjusted by the content of free carbon.
  • the pyrolysis is carried out under a defined hydrogen-containing atmosphere.
  • the concentration of free carbon in the resulting ceramic on the methane gas equilibrium in the corresponding organoelement precursor e.g. Methyl groups as a carbon source
  • carbon fibers or carbon fiber precursor can also improve the electrical or thermal conductivity of a precursor or sintered ceramic.
  • Green body influence is taken on the orientation of the fibers within the resulting ceramic.
  • the fibers are aligned parallel in the flow direction.
  • the thermal and in particular the electrical conductivity of the resulting ceramic is anisotropically adjusted, i. in a based on injection molding ceramics, the properties mentioned in
  • Flow direction of the injection molding higher values than perpendicular to the flow direction.
  • green body materials for the production of carbon fiber-reinforced precursor or sintered ceramics are given below by way of example.
  • the starting materials of precursor ceramics preferably have the following general composition:
  • Carbon fiber precursor fibers of polyvinyl alcohol, phenolic resin, rayon, PAN or mesophase pitch
  • carbon fibers 0-40 vol.%
  • a concrete exemplary embodiment of a carbon-fiber-reinforced precursor ceramic is listed below: 66 vol.% Polysilsesquioxane (MK resin, Wacker AG, Burghausen Germany)
  • Phenolic resin fiber KF-02 BT, Kynol Europa GmbH, Germany
  • the optimum amount of the metal powder, in this case aluminum, in the ceramic starting materials exemplified is determined essentially according to the following connection.
  • the precursor ceramic is deoxygenated so much oxygen that the remaining amount of the elements Si, O and C, which originate from an element-organic precursor, in the precursor ceramic is calculated only as SiO 2 and SiC may be present and thus at least arithmetically no free carbon should exist in the ceramic or even a
  • the preparation of the ceramic starting material is generally carried out by the powdery
  • the mass is preferably prepared in a kneading extruder. Shaping the mass can be done by pressing, transfer molding, injection molding or other plastic molding process. If shaping is performed by hot pressing, this process includes, for example, the following
  • a template is treated with oleic acid as a release agent - Weigh out about 20g of the powdery starting substances into the matrix (5 cm * 5 cm)
  • the molding or the green body is pyrolyzed under an argon atmosphere.
  • the pyrolysis may be listed below, for example
  • Heating rate 100 K / min to 1300 0 C are achieved pyrolysis 2h at 1300 0 C.
  • Cooling rate 300K / min until room temperature is reached
  • a heat treatment in air is preferably carried out for densification and to build up an oxide layer on the precursor ceramic surface. This is done, for example, in compliance with the following parameters:
  • Heating rate: lOOK / min to 1300 0 C are achieved pyrolysis 2h at 1300 0 C.
  • Cooling rate 300K / min until room temperature is reached
  • the starting materials of the corresponding sintered ceramics preferably have the following general composition: 58 - 98 Vol.% Ceramic powder (eg silicon nitride)
  • sintering aid for example yttrium oxide
  • sintering aids such as rare earth compounds or magnesium oxide can also be used.
  • silicon nitride (Grade M II, HCStarck GmbH, Goslar, Germany)
  • the preparation of the ceramic starting material is generally carried out by mixing the powdery starting materials in a ball mill. Subsequently, an injection-moldable starting mixture is produced by adding a suitable polymer as Kohlenstoffmaschineprecursor. For this, the powders and the polymer are kneaded in a kneader under protective gas at about 180 ° C. Thereafter, the shaping takes place by injection molding.
  • thermolysis of the green body thus produced takes place for example in a first step at about 900 0 C in a nitrogen atmosphere.
  • a decomposition of the polymers (debindering) takes place.
  • a pre-sintering takes place.
  • the actual sintering is preferably carried out without pressure in a nitrogen atmosphere at about 1750 0 C for about 2 hours.
  • an optional gas pressure sintering at about 200 bar in a nitrogen atmosphere at about 1900 0 C for approximately 2 hours.
  • the ceramic resistor according to the invention is, for example, as a heating element for
  • Glow plugs, flame candles or ceramic sensor elements suitable and for high temperature applications.

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Abstract

L'invention concerne une résistance céramique pouvant être fabriquée par pyrolyse ou frittage d'un corps de base céramique. Pour de meilleures propriétés mécaniques et/ou électriques, la résistance céramique contient des fibres de carbone.
PCT/EP2006/060896 2005-04-20 2006-03-21 Resistance ceramique et procede de fabrication WO2006111445A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2008507035A JP2008538541A (ja) 2005-04-20 2006-03-21 セラミック抵抗体およびその製造法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102005018268A DE102005018268A1 (de) 2005-04-20 2005-04-20 Keramischer Widerstand und Verfahren zu dessen Herstellung
DE102005018268.2 2005-04-20

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WO2006111445A1 true WO2006111445A1 (fr) 2006-10-26

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DE (1) DE102005018268A1 (fr)
WO (1) WO2006111445A1 (fr)

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GB1264476A (fr) * 1968-07-12 1972-02-23
GB1305910A (fr) * 1969-07-28 1973-02-07
US4540674A (en) * 1983-02-08 1985-09-10 Kyushu Refractories Co., Ltd. Silicon nitride composite refractories
EP0372381A2 (fr) * 1988-12-03 1990-06-13 Hoechst Aktiengesellschaft Procédé pour la production de céramique contenant des fibres
EP0536866A1 (fr) * 1991-10-11 1993-04-14 Noritake Co., Limited Matériau nanocomposite renforcé par fibre de carbone à base de nitrure de silicium et procédé de sa production
EP0623571A1 (fr) * 1992-11-26 1994-11-09 Tonen Corporation Procede pour fabriquer des produits en ceramique
EP1248045A2 (fr) * 2001-04-02 2002-10-09 NGK Spark Plug Company Limited Elément de chauffe en céramique et son procédé de fabrication, bougie de préchauffage et détecteur de courant ionique
EP1496033A2 (fr) * 2003-07-07 2005-01-12 Ngk Insulators, Ltd. Corps fritté en nitrure d'aluminium et son procédé de fabrication
DE10333961A1 (de) * 2003-07-25 2005-02-10 Robert Bosch Gmbh Verfahren zur Herstellung einer Precursor-Keramik

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