METHOD FOR PRODUCING A CONSOLIDATED FIBER PREFORM
20200370170 · 2020-11-26
Inventors
- Thierry Guy Xavier TESSON (MOISSY-CRAMAYEL CEDEX, FR)
- Maxime François Roger CARLIN (MOISSY-CRAMAYEL CEDEX, FR)
- Simon THIBAUD (MOISSY-CRAMAYEL CEDEX, FR)
- Rémy DUPONT (MOISSY-CRAMAYEL CEDEX, FR)
- Ramzi BOHLI (MOISSY-CRAMAYEL CEDEX, FR)
Cpc classification
C23C16/045
CHEMISTRY; METALLURGY
C04B2235/524
CHEMISTRY; METALLURGY
C04B2235/616
CHEMISTRY; METALLURGY
C04B38/066
CHEMISTRY; METALLURGY
C04B35/62897
CHEMISTRY; METALLURGY
C04B35/573
CHEMISTRY; METALLURGY
C23C16/0254
CHEMISTRY; METALLURGY
C04B38/066
CHEMISTRY; METALLURGY
C04B2235/3418
CHEMISTRY; METALLURGY
C04B35/80
CHEMISTRY; METALLURGY
B28B1/52
PERFORMING OPERATIONS; TRANSPORTING
C04B2235/614
CHEMISTRY; METALLURGY
C04B35/80
CHEMISTRY; METALLURGY
International classification
C23C16/04
CHEMISTRY; METALLURGY
B28B1/52
PERFORMING OPERATIONS; TRANSPORTING
C04B35/80
CHEMISTRY; METALLURGY
Abstract
A method for producing a consolidated fiber preform intended for the manufacture of a part made of composite material, includes shaping a fiber texture in a heated metal mold, the texture being pre-impregnated with a transient or fugitive material, or shaping a fiber texture in a metal mold and injecting a transient or fugitive material into the fiber texture held in shape in the metal mold, cooling the mold, removing the set fiber preform from the mold, coating the fiber preform with a slurry containing a powder of ceramic or carbon particles, heat-treating the coated fiber preform so as to form a porous shell around the fiber preform by consolidation of the slurry and so as to remove the transient or fugitive material present in the fiber preform, consolidating the fiber preform by gas-phase chemical infiltration.
Claims
1. A method for producing a consolidated fiber preform intended for the manufacture of a part made of composite material, comprising: shaping a fiber texture in a heated metal mold, the texture being pre-impregnated with a transient or fugitive material, or shaping a fiber texture in a metal mold and injecting a transient or fugitive material into the fiber texture held in shape in the metal mold, cooling the mold, removing the set fiber preform from the mold, coating the fiber preform with a slurry containing a powder of ceramic or carbon particles, heat-treating the coated fiber preform so as to form a porous shell around the fiber preform by consolidation of the slurry and so as to remove the transient or fugitive material present in the fiber preform, and consolidating the fiber preform by gas-phase chemical infiltration.
2. The method according to claim 1, wherein, before the step for consolidating the fiber preform by gas-phase chemical infiltration, piercings are made in the shell.
3. The method according to claim 1, wherein the mold includes a molding cavity having a shape corresponding to the shape of the fiber preform to be produced and one or several channels extending from the molding cavity, the one or several channels being filled with the transient or fugitive material during the injection of the fiber texture into the mold, the transient or fugitive material forming protruding elements on the surface of the preform after removal of said preform, the protruding elements being eliminated during the heat treatment so as to form passage openings in the shell.
4. The method according to claim 1, further comprising, after the step for removing the preform from the mold and before the step for coating the preform with a slurry, forming protruding elements on the surface of the preform.
5. The method according to claim 1, wherein the transient or fugitive material corresponds to a wax to be injected or a transitory resin.
6. The method according to claim 1, wherein the fiber preform is formed by a fiber texture made in a single piece by three-dimensional or multilayer weaving or from a plurality of three-dimensional fiber layers.
7. The method according to claim 1, wherein the fiber texture is made from fibers of silicon carbide, silicon nitride or carbon.
8. The method according to claim 1, wherein the step for consolidation by chemical vapor infiltration of the fiber preform comprises depositing an interphase in the preform, the interphase being made up of one of the following materials: pyrolytic carbon, boron nitride, boron-doped carbon and silicon carbide.
9. A method for manufacturing a part made of composite material comprising producing a consolidated fiber preform according to claim 1, the manufacturing method further comprising, after the step for consolidation by vapor phase infiltration, a step for shaking out the shell, a step for injecting a slurry into the fiber preform and a step for infiltration of the preform with a molten silicon-based composition so as to form a ceramic matrix in said preform.
10. A method for manufacturing a part made of composite material comprising producing a consolidated preform according to claim 1, the manufacturing method further comprising, after the step for consolidation by vapor phase infiltration, a step for injecting a slurry into the fiber preform and a step for infiltration of the preform with a molten silicon-based composition so as to form a ceramic matrix in said preform.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0037] Other features and advantages of the invention will appear upon reading the following description of specific embodiments of the invention, provided as non-limiting examples, in reference to the appended drawings, in which:
[0038]
[0039]
[0040]
[0041]
[0042]
DETAILED DESCRIPTION OF THE INVENTION
[0043] The invention first proposes a method for producing a consolidated fiber preform intended for the manufacture of a part made of ceramic matrix composite (CMC) material, i.e., a material formed by a reinforcement made from carbon or ceramic fibers densified by an at least partially ceramic matrix.
[0044] The inventive method is remarkable in that it does not use graphite conformation tooling in order to consolidate the fiber preform by chemical vapor infiltration. As explained hereinafter in detail and according to the invention, the graphite conformation tooling is replaced by a sacrificial shell formed around the shaped fiber texture, the shell making it possible to maintain the shaping of the fiber texture during its consolidation by chemical vapor infiltration.
[0045] One embodiment of a CMC material according to the inventive method will be described in reference to
[0046] A first step S1 (
[0047] The weaving can be of the interlock type, as illustrated. Other three-dimensional or multilayer weaves can be used, for example multi-cloth or multi-satin weaves. Reference may in particular be made to document WO 2006/136755.
[0048] The fibers making up the fiber texture are preferably ceramic fibers, for example fibers essentially formed by silicon carbide SiC (hereinafter referred to as SiC fiber) or silicon nitride Si.sub.3N.sub.4. It is in particular possible to use SiC fibers marketed under the names Tyranno ZMI, Tyranno Lox-M and Tyranno SA3 by the Japanese company Ube Industries, Ltd or Nicalon,Hi-Nicalon and Hi-Nicalon(S) by the Japanese company Nippon Carbon. In a variant, it is possible to use carbon fibers.
[0049] In a known manner, in the case of ceramic fibers, in particular SiC fibers, a surface treatment of the latter before the formation of an interphase deposit is preferably done to eliminate overspraying and a superficial oxide layer such as silica SiO.sub.2 present on the fibers.
[0050] The following steps consist of maintaining the shaping of the fiber texture in a metal mold 20 and setting the latter to obtain a preform having a shape close to that of the part to be manufactured (
[0051] After cooling of the metal mold, a fiber preform 40 is removed, the preform being set and self-supporting owing to the presence of the transient or fugitive material in solid state therein (step S6,
[0052] The fiber preform 40 thus made is coated with a slurry 50 containing a powder of ceramic or carbon particles (step S7). The powder can be made from one or several of the following elements: oxide-type particles (silica, alumino-silicate, etc.), silicon carbide particles with or without colloidal silica, carbon particles. The coating of the fiber preform can be made by soaking the latter in a slurry bath 50 (
[0053] The fiber preform 40 thus coated by a layer of slurry 50 (
[0054] Vents making it possible to facilitate the discharge of the transient or fugitive material can be arranged in the shell surrounding the preform. These vents can be arranged during the coating of the preform with the slurry by masking certain parts of the preform and forming passages in the shell once the consolidation heat treatment is done. The vents can also be machined in the shell after it is formed. These vents may optionally be plugged up again after the transient or fugitive material is eliminated.
[0055] One thus obtains a preform 80 corresponding to the preform 60 in which the porosity array present between the fibers has been reopened by the removal of the transient or fugitive material, the geometry of the preform 80 in turn being maintained owing to the presence of the shell 60 (
[0056] Optionally, perforations can be made in the shell in order to increase the porosity of the shell and thus facilitate the passage of the infiltration gases (step S9).
[0057] Passage holes can also be made during the formation of the shell. To that end, as illustrated in
[0058] Once the shell is formed, with or without additional perforations or passages, the consolidation is done by vapor phase infiltration of the fiber preform (step S10). To that end, as illustrated in
[0059] The heating in the preheating zone as well as inside the reaction chamber 210 is produced by a graphite susceptor 211 forming an armature electromagnetically coupled with an inductor (not shown).
[0060] The preform 80 is consolidated by chemical vapor infiltration. In order to ensure the consolidation of the preform, a reactive gas containing at least one or several precursors of the material of a consolidation interphase is introduced into the reaction chamber 210. The interphase deposited into the preform can in particular be made from pyrolytic carbon (PyC), or boron nitride (BN), or boron-doped carbon (BC) (with 5 at % to 20 at % boron, the rest being carbon), or silicon carbide. The thickness of the deposited interphase is preferably between 100 nm and 1500 nm. The total thickness of the interphase and the first matrix phase is chosen to be sufficient to consolidate the fiber preform, i.e., to bond the fibers of the preform to one another enough that the preform can be manipulated while preserving its shape without assistance from maintaining tooling. This thickness can be at least equal to 500 nm. After consolidation, the preform remains porous, the initial porosity for example only being filled in for a minority portion by the interphase and the first matrix phase.
[0061] The performance of PyC, BC, B.sub.4C, SiBC, Si.sub.3N.sub.4, BN and SiC depositions by CVI is known. Reference may in particular be made to documents U.S. Pat. Nos. 5,246,736, 5,738,951, 5,965,266, 6,068,930 and 6,284,358.
[0062] Once the consolidation is complete, the shaking out of the shell is done, the latter being destroyed mechanically in order to free, as illustrated in
[0067] In an embodiment variant, the shell can be kept during operations for injecting a slurry and infiltration with a molten silicon-based composition.
[0068] One exemplary embodiment of a consolidated fiber preform intended to manufacture a part made of a CMC composite material according to a method according to the invention is given below: [0069] producing a fiber texture by three-dimensional weaving of the interlock type of SiC fibers, [0070] impregnating the fiber texture with polyvinyl alcohol (PVA), [0071] shaping the fiber texture in a heated metal mold, [0072] cooling the mold, [0073] removing the set fiber preform from the mold, [0074] coating the fiber preform with a slurry containing a mixture of colloidal particles of Sic at 85 at % at SiO.sub.2 at 15 at %, [0075] drying the coated preform at 150 C. for 2 hours, [0076] sintering particles coating the fiber preform at 1000 C. for 1 hour, [0077] consolidating the fiber preform by gas-phase chemical infiltration with or on nitride (BN) deposited therein at a temperature between 700 C. and 900 C.