Polymer-derived ceramic matrix composite components

• US 6,231,793 B1
• Filed: 10/26/1998
• Issued: 05/15/2001
• Est. Priority Date: 10/26/1998
• Status: Expired due to Fees

• Current Assignee: Northrop Grumman Corporation
• Original Assignee: Northrop Grumman Corporation
• Inventors: Strasser, Thomas Edward, Coonce, William Eugene
• Primary Examiner(s): YOON, TAE H
• Application Number:
  US09/178,863
• Time in Patent Office: 932 Days
• Field of Search: 523/149, 523/153, 523/216, 524/401, 264/43, 264/45.1, 264/45.3
• US Class Current: 264/45.1
• CPC Class Codes: C04B 2235/483 Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
• CPC Class Codes: C04B 2235/5224 Alumina or aluminates
• CPC Class Codes: C04B 2235/5228 Silica and alumina, including aluminosilicates, e.g. mullite
• CPC Class Codes: C04B 2235/5232 Silica or silicates other than aluminosilicates, e.g. quartz
• CPC Class Codes: C04B 2235/524 Non-oxidic, e.g. borides, carbides, silicides or nitrides
• CPC Class Codes: C04B 2235/5244 Silicon carbide
• CPC Class Codes: C04B 2235/5248 Carbon, e.g. graphite
• CPC Class Codes: C04B 35/117 Composites
• CPC Class Codes: C04B 35/14 based on silica
• CPC Class Codes: C04B 35/185 Mullite 3Al2O3-2SiO2
• CPC Class Codes: C04B 35/46 based on titanium oxides or titanates containing also zirconium or hafnium oxides, zirconates or hafnates C04B35/49
• CPC Class Codes: C04B 35/528 obtained from carbonaceous particles with or without other non-organic components
• CPC Class Codes: C04B 35/565 based on silicon carbide
• CPC Class Codes: C04B 35/571 obtained from Si-containing polymer precursors or organosilicon monomers
• CPC Class Codes: C04B 35/584 based on silicon nitride
• CPC Class Codes: C04B 35/6269 Curing of mixtures
• CPC Class Codes: C04B 35/62868 Boron nitride
• CPC Class Codes: C04B 35/80 Fibres, filaments, whiskers, platelets, or the like
• CPC Class Codes: C04B 38/0022 obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
• CPC Class Codes: C04B 41/009 characterised by the material treated
• CPC Class Codes: C04B 41/4578 : Coating or impregnating of green ceramics or unset concrete
• CPC Class Codes: C04B 41/459 : Temporary coatings or impregnations C04B40/04 takes precedence
• CPC Class Codes: C04B 41/48 : Macromolecular compounds

Abstract

A method for rapidly manufacturing “green-state” ceramic matrix composite components, components made from this method, and a resin/catalyst precursor mixture used in the method. The method includes manufacturing a component by preparing the precursor mixture by mixing a requisite quantity of a polymer-derived ceramic precursor resin, a catalyst, a discontinuous reinforcing fiber and filler material, and then loading this precursor mixture in a preheated mold. The precursor mixture then is cured in the mold to form the component which is porous. Thereafter, the component is reinfilitrated with a resin to at least partially fill the pores of the component. This method yields a ceramic matrix composite component that is cured in approximately one minute as well as a resin/catalyst precursor mixture that can be stored in excess of four weeks.

Claims

1. A method for fabricating a green state ceramic matrix composite article of manufacture for subsequent pyrolysis, the method comprising the steps of:

a) mixing for mixture formation an amount of a polymer-derived ceramic precursor resin, an amount of a catalyst, discontinuous reinforcing fibers, and a filler material, wherein the amount of precursor resin is between about 50 and 85 volume percent of a theoretically required amount for producing a substantially non-porous green state ceramic matrix composite article of manufacture and wherein the amount of catalyst is between about 4 wt. % and 10 wt. % of the mixture;

b) drying the mixture;

c) preheating a mold having a shape of the article of manufacture to a cure temperature for curing the mixture to a porous green state ceramic matrix composite article of manufacture;

d) placing the mixture into the mold for a period of time sufficient to cure said mixture to said porous green state ceramic matrix composite article of manufacture;

e) ejecting said article of manufacture from the mold; and

f) filling a plurality of pores of said porous green state ceramic matrix composite article of manufacture with said polymer-derived ceramic precursor resin.

2. A method for fabricating a green state ceramic matrix composite article of manufacture as claimed in claim 1 wherein the polymer-derived ceramic precursor resin is polysiloxane resin having an average molecular weight of 1,000.

3. A method for fabricating a green state ceramic matrix composite article of manufacture as claimed in claim 1 wherein the catalyst comprises a siloxane-based monomer having a molecular weight between 200 and 1,000.

4. A method for fabricating a green state ceramic matrix composite article of manufacture as claimed in claim 1 wherein the discontinuous reinforcing fibers are fibers selected from the group consisting of alumina, aluminoborosilicate, aluminum oxide, aluminasilicate, silicon nitride, silicon carbide, silicon carbide, graphite, carbon, peat, and mixtures thereof.

5. A method for fabricating a green state ceramic matrix composite article of manufacture as claimed in claim 1 wherein the filler material is selected from the group consisting of silicon carbide, alumina, mullite, titania, graphite, silicon nitride, silica, and mixtures thereof.

6. A method for fabricating a porous green state ceramic matrix composite article of manufacture for subsequent pore infiltration with polymer-derived ceramic precursor resin and pyrolysis, the method comprising the steps of:

a) mixing for mixture formation an amount of a polymer-derived ceramic precursor resin, an amount of a catalyst, discontinuous reinforcing fibers, and a filler material, wherein the amount of precursor resin is between about 50 and 85 volume percent of a theoretically required amount for producing a substantially non-porous green state ceramic matrix composite article of manufacture and wherein the amount of catalyst is between about 4 wt. % and 10 wt. % of the mixture;

b) drying the mixture;

c) preheating a mold having a shape of the article of manufacture to a cure temperature for curing the mixture to said porous green state ceramic matrix composite article of manufacture;

d) placing the mixture into the mold for a period of time sufficient to cure said mixture to said porous green state ceramic matrix composite article of manufacture; and

e) ejecting said article of manufacture from the mold.

7. A method for fabricating a porous green state ceramic matrix composite article of manufacture as claimed in claim 6 wherein the polymer-derived ceramic percusor resin is polysiloxane resin having an average molecular weight 1000.

8. A method for fabricating a porous green state ceramic matrix composite article of manufacture as claimed in claim 6 wherein the catalyst comprises a siloxane-based monomer having a molecular weight between 200 and 1,000.

9. A method for fabricating a porous green state ceramic matrix composite article of manufacture as claimed in claim 6 wherein the discontinuous reinforcing fibers are fibers selected from the group consisting of alumina, aluminoborosilicate, aluminum oxide, aluminasilicate, silicon nitride, silicon carbide, silicon carbide, graphite, carbon, peat, and mixtures thereof.

10. A method for fabricating a porous green state ceramic matrix composite article of manufacture as claimed in claim 6 wherein the filler material is selected from the group consisting of silicon carbide, alumina, mullite, titania, graphite, silicon nitride, silica, and mixtures thereof.

11. A method for fabricating a green state ceramic matrix composite article of manufacture for subsequent pyrolysis, the method comprising the steps of:

a) mixing for mixture formation

an amount of a polysiloxane ceramic precursor resin having an average molecular weight of 1,000,

an amount of a siloxane-based monomer catalyst having a molecular weight between 200 and 1,000,

discontinuous reinforcing fibers selected from the group consisting of alumina, aluminoborosilicate, aluminum oxide, aluminasilicate, silicon nitride, silicon carbide, silicon carbide, graphite, carbon, peat, and mixtures thereof, and

a filler material selected from the group consisting of silicon carbide, alumina, mullite, titania, graphite, silicon nitride, silica, and mixtures thereof,

wherein the amount of polysiloxane ceramic precursor resin is between about 50 and 85 volume percent of a theoretically required amount for producing a substantially non-porous green state ceramic matrix composite article of manufacture and wherein the amount of siloxane-based monomer catalyst is between about 4 wt. % and 10 wt. % of the mixture;

b) drying the mixture;

c) preheating a mold having a shape of the article of manufacture to a cure temperature for curing the mixture to a porous green state ceramic matrix composite article of manufacture;

d) placing the mixture into the mold for a period of time sufficient to cure said mixture to said porous green state ceramic matrix composite article of manufacture;

e) ejecting said article of manufacture from the mold; and

f) filling a plurality of pores of said porous green state ceramic matrix composite article of manufacture with said polymer-derived ceramic precursor resin.

12. A method for fabricating a porous green state ceramic matrix composite article of manufacture for subsequent pore infiltration with polymer-derived ceramic precursor resin and pyrolysis, the method comprising the steps of:

a) mixing for mixture formation

an amount of a polysiloxane ceramic precursor resin having an average molecular weight of 1,000,

an amount of a siloxane-based monomer catalyst having a molecular weight between 200 and 1,000,

discontinuous reinforcing fibers selected from the group consisting of alumina, aluminoborosilicate, aluminum oxide, aluminasilicate, silicon nitride, silicon carbide, silicon carbide, graphite, carbon, peat, and mixtures thereof, and

a filler material selected from the group consisting of silicon carbide, alumina, mullite, titania, graphite, silicon nitride, silica, and mixtures thereof,

wherein the amount of polysiloxane ceramic precursor resin is between about 50 and 85 volume percent of a theoretically required amount for producing a substantially non-porous green state ceramic matrix composite article of manufacture and wherein the amount of siloxane-based monomer catalyst is between about 4 wt. % and 10 wt. % of the mixture;

b) drying the mixture;

c) preheating a mold having a shape of the article of manufacture to a cure temperature for curing the mixture to a porous green state ceramic matrix composite article of manufacture;

d) placing the mixture into the mold for a period of time sufficient to cure said mixture to said porous green state ceramic matrix composite article of manufacture; and

e) ejecting said article of manufacture from the mold.