Plastic and nonmetallic article shaping or treating: processes – Pore forming in situ – Of inorganic materials
Reexamination Certificate
2000-01-13
2001-06-26
Fiorilla, Christopher A. (Department: 1731)
Plastic and nonmetallic article shaping or treating: processes
Pore forming in situ
Of inorganic materials
C264S642000
Reexamination Certificate
active
06251317
ABSTRACT:
This application claims the benefit of PCT Application Serial No. PCT/SE97/01340, filed Aug. 11, 1997.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The present invention refers to a method of manufacturing a ceramic composite material comprising matrix and reinforcing materials and an intermediate weak interface material, said composite material being particularly intended for use at temperatures above 1400° C. and in an oxidizing environment, the matrix and reinforcing materials consisting of the same or different ceramic oxides having a melting point above 1600° C., and the interface material providing in combination with said materials a stress field liable to micro-cracking.
2. Description of the Related Art
For obtaining an intentional cracking behaviour of such ceramic composites various suggestions have been made, for instance according to WO 93/22258 to the Applicant. In practice, however, it has turned out that an interface layer of ZrO
2
provides a bonding which mostly is too strong. On the other hand, carbon provides a suitably weak bonding between the reinforcing material and the matrix but degrades the fiber material. Over ZrO
2
also HfO
2
fulfills the requirements as to a weak interface zone but in many connections a still weaker interface is desirable.
SUMMARY OF THE INVENTION
Therefore, the main object of the present invention is to suggest a method by which an even weaker interface is obtained. In one aspect of the invention, the reinforcing fiber material is immersed into a powder slurry containing carbon and ZrO
2
so as to be coated thereby and then dried, after which the composite material is subjected to green forming and densification steps as known per se, and finally a heat-treatment in air leaving a porous structure of the interface material. In another aspect of the invention, the reinforcing fiber material is immersed into and coated with a first powder slurry contain WO ing ZrO
2
and then dried and immersed into and coated with a second powder slurry containing carbon and dried, after which the composite material is subjected to green forming and densification steps as known per se, and finally a heat-treatment in air leaving a gap between the reinforcing material and the matrix. It is advantageous to use a powder slurry technique, in which thus rather great particles are used which create a stable porous layer when a coating is used including C/ZrO
2
.
By the present invention it is thus possible to obtain a weak interface securing the necessary crack deflection and fiber pullout behaviour during fracture of the composite.
The coating formed on fibers of which the reinforcing material consist and which are immersed in the slurry has proved to be adherent and strong enough to survive green forming and densification processes. After densification the C is removed by heat treatment in air, leaving a gap or porosity in the oxide interface. The volume fraction of C can be varied to achieve the desired interface strength. The interface made by this invention is stable at high temperatures for long times because the pores have got the right size, i.a. are large enough.
According to the further aspect of the invention, there is provided, however, another way to obtain an interface weak enough, namely to add a fugitive layer. In this method, the reinforcement is first immersed in a C powder slurry, dried and then immersed in an oxide (ZrO
2
) powder slurry, forming a double or sequential coating. Again, this coating is strong and adherent enough to survive green forming and densification. After densification the C is removed by heat treatment leaving a gap between the reinforcing material and the oxide interface. Surface roughness of the reinforcing and matrix materials is sufficient to give load transfer between reinforcing material and matrix material. The absence of bonding between the oxide interface and the reinforcing material will ensure effective crack deflection. The degree of load transfer and frictional sliding resistance between reinforcing material and matrix controlling the fiber pullout behaviour can be varied by varying the thickness of the fugitive C layer.
The presence of an oxide interface will prevent a possible carbothermal reduction of the surface of the reinforcing fiber material of single crystal Al
2
O
3
fibers (to Al
4
C
3
) which would degrade the mechanical properties by defects-created. The presence of oxide interface (especially in the case of a C/ZrO
2
mixture) will locally raise the partial pressure of oxygen and thus prevent the carbothermal reduction to take place.
REFERENCES:
patent: 4732877 (1988-03-01), Olsson et al.
patent: 4885199 (1989-12-01), Corbin et al.
patent: 5290491 (1994-03-01), Heraud et al.
patent: 5622751 (1997-04-01), Thebault et al.
Holmquist Magnus
Lundberg Robert
Molliex Ludovic
Parlier Michel
Parmentier Julien
Fiorilla Christopher A.
Ostrolenk Faber Gerb & Soffen, LLP
Volvo Aero Corporation
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