Vapour phase chemical infiltration process for densifying porous

Coating processes – Coating by vapor – gas – or smoke

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Details

427249, C23C16/26

Patent

active

059049570

DESCRIPTION:

BRIEF SUMMARY
The present invention relates to a chemical vapor infiltration method for densifying porous substrates disposed in annular stacks, i.e. substrates that are substantially bodies of revolution with a central opening or passage and which are disposed in at least one stack defining an interior passage formed by the central openings of the substrates, or substrates that are not necessarily annular in shape, but which are disposed to form a stack with an interior passage defined by the stacked substrates.


BACKGROUND OF THE INVENTION

The field of application of the invention lies in particular in manufacturing composite material parts comprising a porous substrate or "preform" densified by a matrix.
To manufacture composite material parts, in particular thermostructural composite material parts constituted by a refractory fiber preform (e.g. carbon or ceramic fibers) densified by a refractory matrix (e.g. carbon or ceramic), it is common practice to use chemical vapor infiltration methods. Examples of such parts are carbon--carbon (C--C) composite nozzles for thrusters, or C--C composite brake disks, in particular for airplane brakes.
Densifying porous substrates by chemical vapor infiltration consists in placing the substrates in a reaction chamber of an infiltration installation by means of support tooling, and in admitting into the chamber a gas having one or more components constituted by precursors for the material that is to be deposited within the substrates for the purpose of densifying them. Infiltration conditions, in particular gas composition and flow rate, and also temperature and pressure inside the chamber are selected to enable the gas to diffuse within the accessible internal pores of the substrates so that the desired material is deposited therein by a component of the gas decomposing or by a reaction between a plurality of the components thereof.
The conditions required for chemical vapor infiltration of pyrolytic carbon or "pyrocarbon" have been known for a long time to the person skilled in the art. The precursor for carbon is an alkane, an alkyl, or an alkene, generally propane, methane, or a mixture thereof. Infiltration is performed at a temperature of about 1000.degree. C. at a pressure of about 1 kPa, for example. The infiltration conditions required for chemical vapor infiltration of materials other than carbon, in particular ceramic materials, are also well known. On this topic, reference may be made in particular to document FR-A-2 401 888.
In an industrial installation for chemical vapor infiltration, it is usual to load the reaction chamber with a plurality of substrates or preforms to be densified simultaneously, by using support tooling comprising, in particular, trays and spacers. When the preforms are annular, they may be stacked in a longitudinal direction of the reaction chamber. The gas containing the precursor(s) of the material to be deposited within the preforms is admitted at one longitudinal end of the chamber, while the residual gas is evacuated from the opposite end where it is extracted by pumping means. Means are generally provided to preheat the gas before it reaches the preforms to be densified, e.g. means in the form of perforated preheating plates through which the gas passes on being admitted into the reaction chamber.
A real difficulty encountered with known chemical vapor infiltration methods is to ensure that the microstructure of the material deposited within the substrates is constant. In the particular case of composite material parts, the expected properties of said parts require the microstructure of the matrix to be constant and of the kind desired. Thus, in the example of infiltrating pyrolytic carbon or "pyrocarbon", variations in infiltration conditions, even very small variations, can lead to changes in the microstructure of the pyrocarbon. Unfortunately pyrocarbons of the smooth laminar type, of the rough laminar type, and of the isotropic type have properties that are quite distinct. For example, if it is desired to obtain a graphitable pyrocar

REFERENCES:
patent: 5221354 (1993-06-01), Rigney
patent: 5348774 (1994-09-01), Golecki et al.
patent: 5480678 (1996-01-01), Rudolph et al.

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