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Proceedings of International Conference Ceramic Processing Science and Technology, 11-14.09.1994, Friedrichshafen (Germany).

NEW MATERIALS IN THE AlCON - SYSTEM
A. Schneider, R. Schober
Fraunhofer Institute of Ceramic Technologies and Sintered Materials

Poster located on web-site of Fraunhofer Institute of Ceramic Technologies and Sintered Materials

  • Introduction
  • Goal
  • Program
  • Experimental Procedure
  • Experimental Results
  • Conclusions
  • References

  • Introduction

    The recent scientific research in the important field of high temperature corrosive resistant ceramics is connected with the quinary system SiAlCON, in which the SiAlON - system is involved.

    Inside the system there are a lot of possibilities to form solid solutions as part of subsidary quaternary systems in the manner as shown in the rectangles of figure 1.

    FIG. 1: Formation of the solid solutions in the quinary system Si - Al - C - O - N

    FIG. 2: Special interest of this work is directed to the quaternary system Al-C-O-N to improve the high temperature behavior of Al2OC by formation of solid solutions with the isomorphous phase AlN.

    Goal

    Formation, stabilization and characterization of solid solutions of the type (Al2OC)1-x*(AlN)x.

    Program

    In recent years there were published several research results refering to thermodynanics and formation conditions of stabilized Al2OC / 1-5/. Special information and details one can find in the original literature. The aim of this research is to show a suited way to form the solid solution without hygroscopic Al4C3 and to characterize the properties of the (Al2OC)1-x*(AlN)x . The most important steps can be described as following:

    • Investigation of the solid solution formation by reactions according to equation (1) and (2) with AlN - contents from 15 to 70 Mol-%.
    • Sintering in defined CO - and N - atmosphere / 6/.
    • Analytical and x-ray diffractional methods to characterize the solid solution.
    • Measurement of mechanical and physical properties and investigations of the high temperature behavior.

    In this case we favorize raw material mixtures according to field I in figure 3 because of a probable Al2OC formation. Furthermore field II is very interesting because of a low temperature eutectic in the pseudoternary phase diagram Al4C3-Al2O3.

    FIG.3: Favorized areas for the solid solution formation

    Experimental Procedure

    Powders of raw material mixtures:
    AlN: Ventron
    Al2O3: Alcoa, CT 3000
    Al4C3: Fluca, techn., 90%
    Al: Alunova
    C: Thermax No. 991

    Processing / Sintering:
    milling:
    >> dry homogenization, 1 h
    >> ball milling in ethanol, 3h, 500 min-1
    hot pressing conditions:
    > heating rate: 10 Kmin-1
    > temperature: 1800 - 1900°C
    > isotherm periode: 60 min
    > pressure: 30 MPa

    Experimental Results

    It is possible to synthesize a solid solution (Al2OC)1-x*(AlN)x in a wide range of AlN contents, which appears as one phase by x-ray analysis . The x-ray diffraction pattern of a stabilized solid solution with high AlN-content is shown in fig.4. There is no problem to realize the synthesis based on Al and C after equation (2). The typical variation of the lattice constants between those of Al2OC and AlN is demonstrated in table 1 (d-value for (1 0 0)-peak).

    FIG. 4: XRD - pattern of a (Al2OC)1-x * (AlN)x solid solution with 55 Mol-% AlN in raw material mixture.

      Al2OC 25 AlN 45 AlN 55 AlN 55 AlN 70 AlN AlN
    d - value (A) 2,75 2,753 2,740 2,736 2,732 2,724 2,695

    TAB. 1: Typical variation of lattice constants of the solid solutions between those of (Al2OC)1-x * (AlN)x and AlN (peak 1 0 0 ).

    Mechanical and physical properties of the (Al2OC)1-x * (AlN)x solid solution were measured and are shown in table 2. The material appears as typical insulator up to high temperatures.

    TAB. 2: Properties of (Al2OC)1-x * (AlN)x solid solution

    Investigation of wettability:
    The wetting behavior of liquids on solids was investigated in case of liquid steel (9MnNi4) on solid (Al2OC)1-x* (AlN)x compared with the behavior of the test materials BN, SiAlON and SiAlON/Corundum/C - composit (Ar atmosphere, up to 1700°C). In all cases the contact angle (q) shows not wetting but significant differences in stability against reaction with the solid (Tab.2). There was no corrosive attack of molten steel on (Al2OC)1-x*(AlN)x in Ar atmosphere up to 1700°C.
    The investigation was carried out by means of a high temperature microscope of LEICA combined with the measuring system Quantimet 500.

    FIG.6: Investigation of wettability, in fig. B - D is shown the melting of steel on solid (Al2OC)1-x* (AlN)x

    Wettability of (Al2OC)1-x*(AlN)x substrate material in comparison with BN, SiAlON, SiAlON/Corundum/C composit; melting material: steel (9MnNi4); temperature: 25 - 1700 °C; Ar atmosphere

    Conclusions

    Stable (Al2OC)1-x*(AlN)x solid solutions have been verified.
    The substitution of the hygroscopic Al4C3 by Al and C is advantageous for processing.
    The material is applicable for refractories and wear resistant usage (bearings).
    The material indicates the following properties:

    • Electrical non- conductivity (insulator)
    • Thermal conductivity can be influenced by material composition
    • Thermal stability up to 1200 °C (air) for long time applications and for limited time up to 1700 °C (inert atmosphere)
    • Temperature independent bending strength (Sigma bB, 4-p.) up to 1200 °C, SIGMA bB can be increased by optimization of the structure and density.

    References

    1. L.M.Forster, G.Long, M.S.Hunter, Reactions between Aluminum Oxide and Carbon, J.Am.Ceram.Soc., Vol.39, No.1, 1956, pp. 1-11
    2. J.M.Lihrmann, T.Zambetakis, M.Daire, The Aluminum Mono-Oxycarbide Al2OC in the System Si-C-Al-O-N: some thermodynamic properties, J.Am.Ceram.Soc. 72 (9) 1704, 1989
    3. W.Rafaniello, K.Cho, A.V.Virkar, Fabrication and Characterization of SiC-AlN alloys J. Mat.Science 16 (1981) 3479-3488
    4. S.Y.Kuo, A.V.Virkar, Morphology of Phase Separation in AlN-Al2OC and SiC-AlN Ceramics, J.Am.Ceram.Soc., 73 (9) 2640-46, 1990
    5. J.-L.Huang, A.C.Hurford, R.A.Cutler, A.V.Virkar Sintering Behaviour and Properties of SiCAlON ceramics J.Mat.Science 21 (1986) 1448 - 1456
    6. A.Yamaguchi, Affects of Oxygen and Nitrogen Partial Pressure on Stability of Metal, Carbide, Nitride and Oxide in Carbon-Containing Refractories, Taikabutsu Overseas, Vol.7, No.1, pp.4-13

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