EP1704129A1 - Procede de production d'une ceramique-precurseur - Google Patents

Procede de production d'une ceramique-precurseur

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Publication number
EP1704129A1
EP1704129A1 EP04789943A EP04789943A EP1704129A1 EP 1704129 A1 EP1704129 A1 EP 1704129A1 EP 04789943 A EP04789943 A EP 04789943A EP 04789943 A EP04789943 A EP 04789943A EP 1704129 A1 EP1704129 A1 EP 1704129A1
Authority
EP
European Patent Office
Prior art keywords
aluminum
precursor
ceramic
pyrolysis
matrix
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.)
Withdrawn
Application number
EP04789943A
Other languages
German (de)
English (en)
Inventor
Alexander Klonczynski
Ralf Riedel
Martin Koehne
Herwig Schiefer
Rahul Harshe
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.)
Robert Bosch GmbH
Original Assignee
Robert Bosch 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 Robert Bosch GmbH filed Critical Robert Bosch GmbH
Publication of EP1704129A1 publication Critical patent/EP1704129A1/fr
Withdrawn legal-status Critical Current

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/624—Sol-gel processing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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Definitions

  • the invention relates to a method for producing a precursor ceramic according to the preamble of the independent claim.
  • amorphous SiOC ceramics are obtained through the pyrolysis of organic precursors.
  • Advantages of the precursor thermolysis process compared to conventional manufacturing processes for ceramics (sintering) are the significantly lower process temperatures and the easy processability and formability of polysiloxane resins.
  • the electrical and physical property profile of the ceramic composite material of the glow plug resulting after pyrolysis is tailored exactly to the requirement profile.
  • the use of an oxygen-containing polysiloxane precursor as the starting material enables easy processing in air and thus the production of inexpensive products.
  • the pyrolysis product of the filled polysiloxane has good strength, high chemical stability (oxidation, Corrosion) and is harmless to health.
  • one of the great advantages of the precursor thermolysis process over the conventional manufacturing processes (sintering) for ceramic composite materials is the possibility that a larger spectrum of fillers is available.
  • the influence of the matrix on the respective property must be as low as possible. Since the matrix forms a coherent network in all of the composites of the ceramic glow plug, a problem arises for the production of the insulating intermediate layer of the glow plug if the matrix has a too low specific electrical resistance after the production process. Another problem arises in the event that the matrix or the composite loses high-temperature strength and thermal shock resistance due to phase changes, crystallization and oxidation. The problem of the low specific electrical resistance and the undesired crystallization of the matrix material could be significantly reduced by using boron-containing fillers. However, the presence of an amorphous glass can lead to insufficient creep resistance of the matrix material at high temperatures. This can have an effect in particular on the local deformation of the material in the hot areas of the glow pencil.
  • the aim of the present invention is therefore to increase and stabilize the specific electrical resistances of the material used and to achieve an increase in the high-temperature creep resistance.
  • the process according to the invention for the production of precursor ceramics by pyrolysis of oxygen-containing elemental organic precursor polymers has the advantage over the prior art that the resulting material has an increased specific resistance.
  • Another advantage is that the resulting material does not undergo phase changes in the material that lead to its mechanical destruction (durability).
  • an advantage of the method according to the invention is that there is no aging of the specific electrical resistance and therefore no aging of the functional properties of the resulting material.
  • the essence of the invention is the use of aluminum as an additive by modifying the polymer and / or by adding as an additive in the form of aluminum-containing fillers.
  • the modification is a synthesis (for example sol-gel synthesis) of an aluminum-containing polymer.
  • synthesis for example sol-gel synthesis
  • the reaction of the aluminum with the oxygen from the SiOC matrix can be regarded as decisive here. This reaction leads to the formation of a mullite which is significantly more resistant to high temperatures and especially more resistant to high temperatures than amorphous SiOC glass. This improves the durability of the resulting material and the aging of the electrical resistance is reduced.
  • Al C samples There are aluminum-containing SiO (Al) C samples, which were produced either by adding aluminum nanopowder to the polysiloxane or by modifying the polymeric precursors, in an atmosphere intended for the application (i.e., under
  • Argon, H 2 , N 2 , CH 4 , etc. pyrolyzed in the temperature range between 600 ° C - 1400 ° C.
  • the procedure is as follows: In insulation materials, ie materials that are electrically insulating after heat treatment (ceramic materials with a specific electrical resistance R> 10 3 ⁇ cm) or conductive materials, ie materials that are electrically conductive after heat treatment (ceramic materials with a specific electrical resistance R ⁇ 10 ° ⁇ cm), the glow plug is incorporated with aluminum-containing additives during processing.
  • the amount of aluminum incorporated is in the range from 0.1 to 60% by mass, preferably between 0.1 and 5% by mass.
  • the pyrolysis of the insulation materials were all carried out under standard conditions (heating from 20 ° C. to 1300 ° C. at 30 K / h, holding for 1 h at 1300 ° C., and cooling at 300 K / h) in order to compare them with the property profile more conventionally To ensure standard dimensions.
  • Composition 1 65% by volume of polymer (MK-polymer polysilsesquioxane) / 30% by volume of SiO 2/5 vol% aluminum nanopowder mass 2: 65% by volume of polymer (MK-polymer polysilsesquioxane) / 25% by volume of SiO 2 / 10 vol% aluminum nanopowder
  • the masses were prepared by grinding the powders in the planetary ball mill and then sieving them with a mesh size between approximately 100 ⁇ m and approximately 500 ⁇ m. The samples were then shaped and cross-linked using a hot pressing process. The pyrolysis of the samples was carried out at heating rates in the range of 25 K / h in order to ensure compact samples.
  • the pyrolysis was carried out at 1100 ° C, 1200 ° C, 1300 ° C and 1400 ° C.
  • Aluminum-containing conductive masses and insulation masses for a ceramic glow plug with a diameter of approximately 3 mm were produced.
  • the production was carried out by grinding the fillers in the planetary ball mill and then sieving with a mesh size of 150 ⁇ m.
  • the samples were then shaped and crosslinked using a hot press process.
  • the compositions of the ceramic starting materials were in the following range:
  • polysiloxane 50-80% by volume of polysiloxane with an amount of 5% by volume of aluminum nanopowder already contained in the polymer and 1% by weight of zirconium acetylacetonate (based on the amount of polymer) 0-10% by volume SiC 0-20% by volume Al 2 O 3 0-30% by volume MoSi 2 0-5% by mass boron
  • the pyrolysis was carried out with a heating rate of 25K / h to 1300 ° G, an hour of holding time at the final temperature and an argon flow of 2 l / h.
  • the degree of filling in a graphite furnace from FCT was 12%.
  • the samples were then exposed to air in a Nabertherm oven for 8h / 1350 ° C.
  • Insulation material can be stabilized to a value above 10 ohm cm even when aluminum is added. Even after aging at 1350 ° C, no resistance aging can be seen.
  • the very low post-shrinkage of the material after aging at 1350 ° C indicates a significantly higher creep resistance of the matrix material.
  • An aluminum modified resin was made using a sol-gel process.
  • MK polymer with 1% by mass of zirconium acetylacetonate as catalyst was dissolved in isopropanol and a proportion of 9.1% by mass of alumatran (AKA005 from ABCR) (based on the polymer) was added. After gelling, the gel was dried at 120 ° C for 5 hours.
  • the dried gel was then ground and then hot pressed at 180 ° C.
  • Pyrolysis temperature was 1100 ° C in an argon atmosphere.
  • the glass transition temperature of aluminosilicate glasses is T> 1500 ° C and thus at least 150 ° C higher than that of SiO 2 or borosilicate glasses.
  • the achievable strength level of a mullite / SiC composite is considerably higher (approximately 400 MPa) than that of pure SiOC ceramics (approximately 150 MPa).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Structural Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Combustion & Propulsion (AREA)
  • Composite Materials (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Ceramic Products (AREA)

Abstract

L'invention concerne un procédé de production d'une céramique-précurseur par pyrolyse de polymères précurseurs organométalliques oxygénés. Les précurseurs polymères contiennent de l'aluminium comme additif.
EP04789943A 2003-12-09 2004-10-08 Procede de production d'une ceramique-precurseur Withdrawn EP1704129A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2003157354 DE10357354A1 (de) 2003-12-09 2003-12-09 Verfahren zur Herstellung einer Precursor-Keramik
PCT/DE2004/002234 WO2005056494A1 (fr) 2003-12-09 2004-10-08 Procede de production d'une ceramique-precurseur

Publications (1)

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EP1704129A1 true EP1704129A1 (fr) 2006-09-27

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EP04789943A Withdrawn EP1704129A1 (fr) 2003-12-09 2004-10-08 Procede de production d'une ceramique-precurseur

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EP (1) EP1704129A1 (fr)
DE (1) DE10357354A1 (fr)
WO (1) WO2005056494A1 (fr)

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5635250A (en) * 1985-04-26 1997-06-03 Sri International Hydridosiloxanes as precursors to ceramic products
US5418298A (en) * 1993-03-19 1995-05-23 Regents Of The University Of Michigan Neutral and mixed neutral/anionic polymetallooxanes
DE10055082A1 (de) * 2000-11-07 2002-05-16 Bosch Gmbh Robert Keramischer Verbundwerkstoff

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2005056494A1 *

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DE10357354A1 (de) 2005-07-07
WO2005056494A1 (fr) 2005-06-23

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