CN107188590B - Forming method of fiber reinforced SiC-based composite material - Google Patents
Forming method of fiber reinforced SiC-based composite material Download PDFInfo
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- C04B35/571—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained from Si-containing polymer precursors or organosilicon monomers
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Abstract
The invention belongs to the technical field of preparation of ceramic matrix composites, and relates to a forming method of a fiber reinforced SiC matrix composite. The invention adopts a mode of combining the first period metal injection mold molding and the densification period graphite cracking mold molding to ensure that the fiber reinforced SiC-based composite material is molded in a near net size in the whole PIP process. Firstly, preparing a fiber preform by taking fibers as raw materials, placing the fiber preform in a graphite mold for preforming, transferring the fiber preform to a metal injection mold for primary cycle molding by using a solvent-free liquid state, and finally, carrying out densification cycle molding on the fiber reinforced SiC-based composite material in a graphite cracking mold with holes by adopting a precursor impregnation pyrolysis process (PIP). The method can realize the near net size molding of the fiber reinforced SiC-based composite material, the prepared material has high dimensional precision, the processing cost is saved, the processing period is shortened, and the engineering process of the ceramic-based composite material is promoted.
Description
Technical Field
The invention belongs to the technical field of preparation of ceramic matrix composites, and relates to a forming method of a fiber reinforced SiC matrix composite.
Background
The ceramic matrix composite not only retains the excellent performances of high temperature resistance, low density, high specific strength, high specific modulus, oxidation resistance, ablation resistance and the like of the ceramic material, but also overcomes the fatal defects of high brittleness, poor reliability and the like of the ceramic material, and has the characteristics of similar metal fracture behavior, insensitivity to cracks, no catastrophic damage and the like. The fiber reinforced SiC-based composite material has the characteristics of high temperature resistance, low density, oxidation resistance and the like, is a key point of domestic and foreign research, and has wide application prospects in the fields of aviation, aerospace and the like. At present, the hot point of domestic and foreign research is the molding technology and the preparation process of the fiber reinforced SiC-based composite material.
The precursor impregnation pyrolysis process (PIP) is one of the ceramic matrix composite preparation processes which are researched more and developed rapidly in recent years. The PIP process for preparing ceramic matrix composite uses a fiber preform as a framework, firstly, the fiber preform is dipped in a polymer precursor, air in the fiber preform is removed, the fiber preform is filled after solution crosslinking curing or solvent volatilization, then, the fiber preform is pyrolyzed under the protection of inert atmosphere, and finally, the polymer is converted into ceramic. The PIP process has the advantages that: the base material with controllable components can be prepared through the component design of the precursor; the cracking temperature is lower, and the damage to the fiber in the heat treatment process is reduced.
At present, the PIP process generally uses solid Polycarbosilane (PCS) as a precursor, the solid PCS is used as an impregnant after being dissolved by a solvent during impregnation, and due to the existence of the solvent, the composite material can be molded only by a hot press, but a closed metal injection mold molding mode cannot be adopted, so that the defects of poor molding property and the like of the composite material are caused; in addition, as the commonly used solid PCS cannot generate crosslinking curing reaction during heating, the size of the composite material is seriously changed during cracking in a high-temperature furnace, the material molding is incomplete, the subsequent processing workload is large, and the processing cost is high.
Disclosure of Invention
The invention aims to provide a method for molding a fiber reinforced SiC-based composite material, which has small size change, small subsequent processing amount and low processing cost in the molding process of the composite material.
The technical scheme of the invention is that the forming method of the fiber reinforced SiC-based composite material comprises the following steps:
step one, performing a fiber preform; preparing a fiber preform by taking fibers as a raw material, and ensuring that the volume fraction of the fibers is 40-50%; placing the fiber preform in a graphite mold, and performing the fiber preform by using a hot press;
step two, the fiber reinforced SiC-based composite material is molded in a first period; packaging the fiber preform into a metal injection mold, adopting a solvent-free liquid polycarbosilane precursor as injection resin, performing vacuum and pressure injection at the pressure speed of 0.05-0.10 MPa/10-60 min to 0.20-0.40 MPa, placing the fiber preform and the metal injection mold in an oven for curing after the injection is finished, taking out the fiber reinforced SiC-based composite material blank from the metal injection mold after the curing is finished, and transferring the fiber reinforced SiC-based composite material blank into a graphite cracking mold with holes;
step three, performing densification cycle molding on the fiber reinforced SiC-based composite material; placing the fiber reinforced SiC-based composite material blank formed in the first period and a graphite cracking mold with holes into a high-temperature furnace at 800-1600 ℃ for cracking, preserving the heat for 1-2h, and cooling to room temperature; then, putting the fiber reinforced SiC-based composite material blank and a graphite cracking mould with holes into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and dipping, keeping the vacuum degree at 0.1 +/-0.01 MPa for 6-12 h, taking out, cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the graphite cracking mould with holes, putting the fiber reinforced SiC-based composite material blank and the graphite cracking mould with holes into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 3-5 times, taking out the fiber reinforced SiC-based composite material blank from the graphite cracking mould with holes, putting the blank into the closed container containing the solvent-free liquid polycarbosilane precursor, vacuumizing and dipping, keeping the vacuum degree at 0.1 +/-0.01 MPa for 6-12 h, taking out, cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the fiber reinforced SiC-based composite material blank, and placing the fiber reinforced SiC-based composite material blank into a graphite cracking die with holes, placing the fiber reinforced SiC-based composite material blank and the graphite cracking die with the holes into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 5-10 times until the weight of the cracked fiber reinforced SiC-based composite material blank is increased by less than 2%, and completing the densification cycle molding of the fiber reinforced SiC-based composite material.
The method comprises the steps of preforming a fiber preform by using a hot press, preforming the fiber preform by using the hot press, laying the fiber preform in a graphite mold, heating the hot press to 100-300 ℃, keeping the temperature for 0.5-1 h, then placing the graphite mold in the middle of a working area of the hot press, pressurizing, keeping the pressure at 1-2 MPa, and cooling to room temperature after keeping the temperature for 2-10 h.
The metal injection mold body formed by the fiber reinforced SiC-based composite material in the first period comprises a female mold, a male mold and a cushion frame, and also comprises a mold frame and a mold base besides the mold body; punching glue holes on the female die, wherein the hole diameter is 2-6 mm, the hole interval is 30-50 mm, punching glue holes on one side of the male die, the hole diameter is 2-6 mm, and the metal injection die is made of steel; the solvent-free liquid polycarbosilane precursor is used as injection resin, and the viscosity of the solvent-free liquid polycarbosilane precursor is 20-200 mPa & s at 25 ℃.
The first cycle molding method of the fiber reinforced SiC based composite material may be,
flatly placing the fiber preform in a metal injection mold cavity, plugging a proper amount of putty strips at the edge of an end head, installing silica gel strips, and assembling a mold; connecting a glue inlet of the metal injection mould with a glue outlet of the glue injection tank, and connecting the glue outlet of the metal injection mould with a vacuum system; vacuumizing, and checking the vacuum degree of the mold, wherein the vacuum degree is required to be kept above 0.080MPa for 20 min; degassing the resin in vacuum, wherein the vacuum pressure difference is not lower than 0.080MPa, the degassing time is 30-60 min, and the resin is injected for 10-60 min in a vacuum state; connecting compressed gas, keeping the pressure at 0.05 + -0.01 MPa, and injecting; closing all glue outlet valves after the glue outlet of the glue outlet is stable, and keeping the pressure for 10-60 min; gradually increasing the injection pressure at a speed of 0.05-0.10 MPa every 10-60 min, and after all glue outlets discharge glue, completely closing the valves and keeping the pressure for 10-60 min; the highest pressure is not more than 0.40 MPa;
and after the injection is finished, putting the fiber preform and the metal injection mold into an oven for curing, wherein the curing temperature is 200-400 ℃, and the curing and heat preservation time is 2-4 h. After the solidification is finished, cooling the metal injection mold along with the oven;
and (3) cooling the temperature of the metal injection mold to below 40 ℃, opening the mold, taking out the cured fiber reinforced SiC-based composite material blank, and transferring the blank into a graphite cracking mold with holes for fixing.
The advantages and the beneficial effects of the invention are that,
the invention realizes a molding method of a fiber reinforced SiC-based composite material for the first time, a fiber reinforced SiC-based composite material part prepared by the method can achieve near net size molding, the thickness of a fiber preform, a solidified blank and a densified blank of the fiber reinforced SiC-based composite material prepared by the method is increased by no more than 5%, compared with other molding methods of the fiber reinforced SiC-based composite material, the fiber and a matrix can be fully utilized, and the number of paving layers of the ceramic-based composite material obtained by the theoretical calculation of fiber volume fraction is more consistent with the actual material; because the fiber reinforced SiC-based composite material part prepared by the method has high dimensional accuracy, the material has small later-stage processing allowance, only needs to be ground, saves the processing cost, shortens the processing period and promotes the engineering process of the ceramic-based composite material.
The solvent-free liquid polycarbosilane is used as an impregnant for the PIP process, so that the solvent-free liquid polycarbosilane ceramic has high yield, a macromolecular three-dimensional network structure can be formed during heating, volatilization of organic micromolecules is reduced, collapse and deformation of a fiber preform in the PIP process forming process can be avoided, and the application of the solvent-free liquid polycarbosilane can shorten the preparation period of a composite material and promote the application of a fiber reinforced ceramic matrix composite material while realizing near net size forming of the fiber reinforced SiC matrix composite material; secondly, the solvent-free liquid polycarbosilane is used as an impregnant of the PIP process, no toxic and harmful gas is discharged in the forming process of the fiber reinforced SiC-based composite material, and the process is safer and more environment-friendly; thirdly, the impregnant used in the traditional PIP process contains a large amount of solvent and cannot be molded in a closed metal mold, so that the dimensional accuracy is poor, the solvent-free liquid polycarbosilane does not contain solvent, and the use of the impregnant makes it possible to perform first cycle curing molding on the fiber reinforced SiC-based composite material by using a metal injection mold.
According to the invention, the metal injection mold is used for carrying out primary cycle curing molding on the fiber reinforced SiC-based composite material, the molding of a workpiece with a complex shape can be realized by designing the shape, the size, the glue inlet and outlet and the flow channel of the metal injection mold, and compared with the traditional PIP process in which a graphite mold is adopted for molding, the shape and the thickness of the composite material are accurately controlled; in addition, the metal injection mold can be recycled for a long time, and the manufacturing cost of the tool is saved.
The graphite cracking mould with the holes is used as the mould for the densification cycle forming of the fiber reinforced SiC-based composite material, so that the non-demoulding of the impregnation-cracking process can be realized, the deformation of the fiber reinforced SiC-based composite material in the demoulding-mould closing process is reduced, and the control of the material size, particularly the thickness, is more accurate.
In conclusion, the thickness of the prepared fiber reinforced SiC-based composite material part can be accurately controlled by innovating a PIP process forming mode, the loss of a fiber preform is reduced, the later-stage processing cost is reduced, and the method has wide market popularization and application prospects.
Drawings
FIG. 1 is a schematic view of the first-cycle metal injection molding of the fiber reinforced SiC-based composite material of the present invention;
FIG. 2 is a schematic view of the forming in a graphite cracking mold with a porous fiber reinforced SiC-based composite material densification period according to the present invention;
FIG. 3 is a thickness variation diagram of a SiC fiber reinforced SiC-based composite material during the process of forming a flat plate according to an embodiment of the present invention;
FIG. 4 is a thickness variation diagram of a second C fiber reinforced SiC-based composite material flat plate forming process according to an embodiment of the present invention;
fig. 5 is a thickness variation diagram of an arc-shaped workpiece made of three SiC fiber reinforced SiC based composites according to an embodiment of the present invention.
Detailed Description
The following detailed description of the embodiments of the present invention is provided in conjunction with the accompanying drawings to enable those skilled in the art to more clearly understand the present invention, but not to limit the scope of the present invention.
The molding method of a fiber-reinforced SiC-based composite material according to the present invention is described below:
step one, performing a fiber preform; preparing a fiber preform by taking fibers as a raw material, and ensuring that the volume fraction of the fibers is 40-50%; placing the fiber preform in a graphite mold, and performing the fiber preform by using a hot press;
step two, the fiber reinforced SiC-based composite material is molded in a first period; packaging the fiber preform into a metal injection mold, adopting a solvent-free liquid polycarbosilane precursor as injection resin, performing vacuum and pressure injection at the pressure speed of 0.05-0.10 MPa/10-60 min to 0.20-0.40 MPa, placing the fiber preform and the metal injection mold in an oven for curing after the injection is finished, taking out the fiber reinforced SiC-based composite material blank from the metal injection mold after the curing is finished, and transferring the fiber reinforced SiC-based composite material blank into a graphite cracking mold with holes;
step three, performing densification cycle molding on the fiber reinforced SiC-based composite material; placing the fiber reinforced SiC-based composite material blank formed in the first period and a graphite cracking mold with holes into a high-temperature furnace at 800-1600 ℃ for cracking, preserving the heat for 1-2h, and cooling to room temperature; then, putting the fiber reinforced SiC-based composite material blank and a graphite cracking mould with holes into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and dipping, keeping the vacuum degree at 0.1 +/-0.01 MPa for 6-12 h, taking out, cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the graphite cracking mould with holes, putting the fiber reinforced SiC-based composite material blank and the graphite cracking mould with holes into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 3-5 times, taking out the fiber reinforced SiC-based composite material blank from the graphite cracking mould with holes, putting the blank into the closed container containing the solvent-free liquid polycarbosilane precursor, vacuumizing and dipping, keeping the vacuum degree at 0.1 +/-0.01 MPa for 6-12 h, taking out, cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the fiber reinforced SiC-based composite material blank, and placing the fiber reinforced SiC-based composite material blank into a graphite cracking die with holes, placing the fiber reinforced SiC-based composite material blank and the graphite cracking die with the holes into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 5-10 times until the weight of the cracked fiber reinforced SiC-based composite material blank is increased by less than 2%, and completing the densification cycle molding of the fiber reinforced SiC-based composite material.
The weaving mode of the fiber preform in the first step can be two-dimensional weaving, 2.5-dimensional weaving, three-dimensional weaving and the like.
And step one, performing the fiber preform by using a hot press, performing the fiber preform by using the hot press, laying the fiber preform in a graphite mold, heating the hot press to 100-300 ℃, keeping the temperature for 0.5-1 h, then placing the graphite mold in the middle of a working area of the hot press, pressurizing, keeping the pressure at 1-2 MPa, and cooling to room temperature after keeping the temperature for 2-10 h.
Step one the graphite mold may be a graphite mold with holes or a graphite mold without holes.
Step two, the metal injection mold body of the fiber reinforced SiC-based composite material formed in the first period comprises a female mold, a male mold and a cushion frame, and also comprises a mold frame and a mold base besides the mold body; punching glue holes on the female die, wherein the hole diameter is 2-6 mm, the hole interval is 30-50 mm, punching glue holes on one side of the male die, the hole diameter is 2-6 mm, and the metal injection die is made of steel; the solvent-free liquid polycarbosilane precursor is used as injection resin, and the viscosity of the solvent-free liquid polycarbosilane precursor is 20-200 mPa & s at 25 ℃.
The first period molding method of the fiber reinforced SiC based composite material in the second step may be,
flatly placing the fiber preform in a metal injection mold cavity, plugging a proper amount of putty strips at the edge of an end head, installing silica gel strips, and assembling a mold; connecting a glue inlet of the metal injection mould with a glue outlet of the glue injection tank, and connecting the glue outlet of the metal injection mould with a vacuum system; vacuumizing, and checking the vacuum degree of the mold, wherein the vacuum degree is required to be kept above 0.080MPa for 20 min; degassing the resin in vacuum, wherein the vacuum pressure difference is not lower than 0.080MPa, the degassing time is 30-60 min, and the resin is injected for 10-60 min in a vacuum state; connecting compressed gas, keeping the pressure at 0.05 + -0.01 MPa, and injecting; closing all glue outlet valves after the glue outlet of the glue outlet is stable, and keeping the pressure for 10-60 min; gradually increasing the injection pressure at a speed of 0.05-0.10 MPa every 10-60 min, and after all glue outlets discharge glue, completely closing the valves and keeping the pressure for 10-60 min; the highest pressure is not more than 0.40 MPa;
and after the injection is finished, putting the fiber preform and the metal injection mold into an oven for curing, wherein the curing temperature is 200-400 ℃, and the curing and heat preservation time is 2-4 h. After the solidification is finished, cooling the metal injection mold along with the oven;
and (3) cooling the temperature of the metal injection mold to below 40 ℃, opening the mold, taking out the cured fiber reinforced SiC-based composite material blank, and transferring the blank into a graphite cracking mold with holes for fixing.
The compressed gas in the second step can be compressed air, nitrogen and argon.
And step three, after the densification cycle molding of the fiber reinforced SiC-based composite material is completed, machining the fiber reinforced SiC-based composite material if necessary, and carrying out ultrasonic cleaning and drying treatment on the machined fiber reinforced SiC-based composite material.
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
In the embodiment, 1K SiC fiber is used as a raw material, solvent-free liquid polycarbosilane is used as a precursor, a perforated graphite cracking mold is used as a mold for performing and densifying the fiber preform for periodic molding, a metal injection mold is used as a first periodic molding mold, and finally a precisely-molded SiC fiber reinforced SiC-based composite flat plate (hereinafter referred to as a SiC/SiC flat plate) is obtained, wherein the flat plate has the length of 100mm, the width of 100mm and the thickness of 3mm, and comprises the following steps:
1K SiC fiber is used as a raw material, a two-dimensional weaving and layering mode is adopted to prepare a SiC fiber preform, and the volume fraction of the fiber is 45%.
The graphite cracking mould with holes is used for processing the preforming and the densification cycle forming of the SiC/SiC flat plate preform, through holes are punched on the graphite cracking mould, the aperture is 2mm, the hole spacing is 6mm, the holes are uniformly distributed, and the graphite material is high-strength graphite.
And placing the SiC fiber preform after laying in a perforated graphite cracking mold, and fixing the perforated graphite cracking mold.
Performing SiC/SiC plate fiber preforms by using a hot press, laying the SiC/SiC fiber preforms in a graphite cracking mould with holes, heating the hot press to 150 ℃, keeping the temperature for 1 hour, then placing the graphite cracking mould with the holes in the middle of a working area of the hot press, pressurizing to 1Mpa, keeping the temperature for 2 hours, and cooling to room temperature.
The first cycle of processing is metal injection mould for shaping, and the mould size is long 120mm, and wide 120mm, fills up frame thickness 3mm, beats 2 and goes out the gluey hole on the bed die, and the aperture is 2mm, and the hole interval is 30mm, goes out gluey hole and is located bed die one side, beats a hole of advancing gluey in the middle of the bed die one side, and the aperture is 3mm, and metal injection mould material is the steel.
The solvent-free liquid polycarbosilane precursor is used as injection resin, the solvent-free liquid polycarbosilane precursor is a light yellow liquid at normal temperature, has no solvent and has viscosity of 24mPa & s at 25 ℃, and is provided by Chinese academy chemistry.
Before use, the solvent-free liquid polycarbosilane is put into a glue injection tank, and vacuum defoamation is carried out for 40min, wherein the vacuum degree is 0.095MPa during vacuum defoamation.
Flatly placing the preformed SiC/SiC plate fiber preform in a cavity of a metal injection mold, plugging a proper amount of putty strips at the edge of an end head, installing silica gel strips, and assembling the mold; connecting a glue inlet of the metal injection mould with a glue outlet of the glue injection tank, and connecting the glue outlet of the metal injection mould with a vacuum system; vacuumizing, and checking the vacuum degree of the metal injection mold, wherein the vacuum degree is maintained for 20min at more than 0.085 MPa.
Injecting the resin for about 10min in a vacuum state, and after the injection is finished in the vacuum state, switching on nitrogen, keeping the air pressure at 0.05MPa, and injecting; closing all glue outlet valves after the glue outlet of the glue outlet is stable, and keeping the pressure for 10 min; gradually increasing the injection pressure at a speed of 0.05MPa every 10min, completely closing the valves after all the glue outlets discharge glue, and keeping the pressure for 20 min; the highest injection pressure is 0.30 MPa.
And after the injection is finished, putting the fiber preform and the metal injection mold into an oven for curing at the curing temperature of 240 ℃ for 3 h. After curing is complete, the metal injection mold is cooled with the oven.
And (3) opening the die when the temperature of the metal injection die is reduced to 30 ℃, taking out the cured SiC/SiC flat plate, transferring the cured SiC/SiC flat plate blank into a graphite cracking die with holes for fixing, wherein the average thickness of the cured SiC/SiC flat plate blank is 3.02mm and is 0.6% of the target size deviation.
And putting the cured SiC/SiC flat plate blank together with the perforated graphite cracking mould into a high-temperature furnace at 800-1600 ℃ for cracking, wherein the cracking temperature is 1000 ℃, the heat preservation time is 1h, and the pressure is normal pressure.
And after cracking, taking the SiC/SiC flat plate blank together with the perforated graphite cracking mould out of a high-temperature furnace at 800-1600 ℃, putting the blank into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and dipping the container at a vacuum degree of-0.1 MPa for 6 hours, and taking out the blank and cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the perforated graphite cracking mould.
Putting the SiC/SiC flat plate blank and the perforated graphite cracking mould into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 3 times, taking the SiC/SiC flat plate blank out of the perforated graphite cracking mould, putting the blank into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and impregnating, keeping the vacuum degree at 0.095MPa for 6h, taking out, cleaning a residual solvent-free liquid polycarbosilane precursor on the surface of the SiC/SiC flat plate blank, placing the SiC/SiC flat plate blank in a perforated graphite cracking mold, placing the SiC/SiC flat plate blank and the perforated graphite cracking mold in a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the impregnation-cracking process for 7 times, increasing the weight of the SiC/SiC flat plate blank by 0.91% after cracking for the 10 th time, and completing the periodic densification molding of the SiC/SiC flat plate.
And taking the SiC/SiC flat plate out of the graphite cracking mould with the hole, wherein the average thickness of the SiC/SiC flat plate is 3.1mm after the SiC/SiC flat plate is taken out, and the thickness is 3% thicker than the target size, so that the molding of the SiC/SiC flat plate is completed.
Example 1 a SiC/SiC flat plate having dimensions of 100mm in length, 100mm in width and 3.1mm in thickness was produced, the thickness was increased by only 3% compared to the target dimension, and the thickness change during the forming process is shown in fig. 3.
Example 2
In the embodiment, T300C fiber is used as a raw material, solvent-free liquid polycarbosilane is used as a precursor, a graphite mold without holes is used as a fiber preform preforming mold, a graphite cracking mold with holes is used as a densification period forming mold, a metal injection mold is used as a first period forming mold, and finally, a precisely formed C fiber reinforced SiC-based composite material flat plate (hereinafter referred to as a C/SiC flat plate) is obtained, wherein the flat plate has the length of 200mm, the width of 200mm and the thickness of 4mm, and the method comprises the following steps:
the method is characterized in that T300C fiber is used as a raw material, a C fiber preform is prepared in a two-dimensional weaving and layering mode, and the volume fraction of the fiber is 40%.
Processing a graphite mould for preforming a C/SiC plate fiber preform, processing a graphite cracking mould with holes for forming a densification cycle of a C/SiC plate, punching through holes on the graphite cracking mould, wherein the hole diameter is 4mm, the hole spacing is 8mm, the holes are uniformly distributed, and the graphite material is high-strength graphite.
And placing the C fiber preform after laying in a graphite cracking mould with holes, and fixing the graphite cracking mould with the holes.
Performing the C/SiC flat fiber preform by using a hot press, laying the C/SiC fiber preform in a graphite cracking die with holes, heating the hot press to 200 ℃, keeping the temperature for 0.5h, then placing the graphite cracking die with the holes in the middle of a working area of the hot press, pressurizing to 1.5Mpa, preserving the heat for 3h, and cooling to room temperature.
The first cycle of processing is metal injection mould for shaping, and the mould size is long 250mm, wide 250mm, fills up frame thickness 4mm, beats 6 and goes out the gluey hole on the bed die, and the aperture is 5mm, and the hole interval is 40mm, goes out gluey hole and is located bed die one side, beats a gluey hole of advancing in the middle of the bed die one side, and the aperture is 5mm, and metal injection mould material is the steel.
The solvent-free liquid polycarbosilane precursor is used as injection resin, the solvent-free liquid polycarbosilane precursor is orange liquid at normal temperature, has no solvent, has viscosity of 138 mPa.s at 25 ℃, and is provided by the chemical industry of Chinese academy of sciences.
Before use, the solvent-free liquid polycarbosilane is put into a glue injection tank, and vacuum defoamation is carried out for 1h, wherein the vacuum degree is 0.095MPa during vacuum defoamation.
Flatly placing the preformed C/SiC plate fiber preform in a metal injection mold cavity, plugging a proper amount of putty strips at the edge of an end head, installing silica gel strips, and assembling a mold; connecting a glue inlet of the metal injection mould with a glue outlet of the glue injection tank, and connecting the glue outlet of the metal injection mould with a vacuum system; vacuumizing, and checking the vacuum degree of the metal injection mold, wherein the vacuum degree is maintained at 0.085MPa for 20 min.
Injecting the resin for about 20min in a vacuum state, and after the injection is finished in the vacuum state, connecting compressed air, keeping the air pressure at 0.05MPa, and injecting; closing all glue outlet valves after the glue outlet of the glue outlet is stable, and keeping the pressure for 20 min; gradually increasing the injection pressure at a speed of 0.05MPa every 20min, completely closing the valves after all the glue outlets discharge glue, and keeping the pressure for 30 min; the highest injection pressure is 0.35 MPa.
And after the injection is finished, putting the fiber preform and the metal injection mold into an oven for curing at the curing temperature of 200 ℃ for 4 h. After curing is complete, the metal injection mold is cooled with the oven.
And (3) opening the mold when the temperature of the metal injection mold is reduced to 25 ℃, taking out the cured C/SiC flat plate, transferring the cured C/SiC flat plate blank into a graphite cracking mold with holes for fixing, wherein the average thickness of the cured C/SiC flat plate blank is 4.05mm and is 1.2% of the target size deviation.
And putting the cured C/SiC flat plate blank together with the perforated graphite cracking mould into a high-temperature furnace at 800-1600 ℃ for cracking, wherein the cracking temperature is 1200 ℃, the heat preservation time is 1h, and the pressure is normal pressure.
And after cracking, taking the C/SiC flat plate blank together with the perforated graphite cracking mould out of a high-temperature furnace at 800-1600 ℃, putting the C/SiC flat plate blank into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and dipping the container at a vacuum degree of-0.1 MPa, keeping the vacuum degree for 8 hours, and taking out the C/SiC flat plate blank and the perforated graphite cracking mould to clean the residual solvent-free liquid polycarbosilane precursor on the surface of the perforated graphite cracking mould.
Putting the C/SiC flat plate blank and the perforated graphite cracking mould into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 4 times, taking the C/SiC flat plate blank out of the perforated graphite cracking mould, putting the C/SiC flat plate blank into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and dipping, keeping the vacuum degree at 0.1MPa for 8h, taking out, cleaning a residual solvent-free liquid polycarbosilane precursor on the surface of the C/SiC flat plate blank, placing the C/SiC flat plate blank in a perforated graphite cracking mould, placing the C/SiC flat plate blank and the perforated graphite cracking mould in a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 6 times, increasing the weight of the C/SiC flat plate by 0.80% after cracking for 10 times, and completing the densification cycle molding of the C/SiC flat plate.
And taking the C/SiC flat plate out of the graphite cracking mould with the hole, wherein the average thickness of the C/SiC flat plate is 4.18mm after the C/SiC flat plate is taken out, and the C/SiC flat plate is thickened by 4.5% compared with the target size. And finishing the molding of the C/SiC flat plate.
Example 2 the thickness variation during the forming process is shown in figure 4.
Example 3
In the embodiment, 1K SiC fiber is used as a raw material, solvent-free liquid polycarbosilane is used as a precursor, a perforated graphite cracking mold is used as a mold for performing and periodic densification molding of a fiber preform, a metal injection mold is used as a first period molding mold, and finally, an accurately molded SiC fiber reinforced SiC-based composite arc-shaped part is obtained, wherein the length of the part is 280mm, the width of the part is 120mm, and the thickness of the part is 5mm, and the method comprises the following steps:
1K SiC fiber is used as a raw material, a 2.5D weaving mode is adopted to prepare a SiC fiber preform, and the volume fraction of the fiber is 50%.
The graphite cracking mould with holes is used for processing the preforming and densification cycle forming of the SiC/SiC arc-shaped workpiece, through holes are punched in the graphite cracking mould, the aperture is 5mm, the hole spacing is 6mm, the holes are uniformly distributed, and the graphite material is high-strength graphite.
And placing the SiC arc-shaped workpiece fiber preform after laying in a graphite cracking mould with holes, and fixing the graphite cracking mould with the holes.
Performing the SiC/SiC arc-shaped part fiber preform by using a hot press, laying the SiC/SiC arc-shaped part fiber preform in a graphite cracking die with holes, heating the hot press to 300 ℃, keeping the temperature for 1h, then placing the graphite cracking die with the holes in the middle of a working area of the hot press, pressurizing to 1.5Mpa, preserving the heat for 5h, and cooling to room temperature.
The first cycle of processing is metal injection mould for shaping, and the mould size is long 320mm, and is wide 180mm, fills up frame thickness 5mm, beats 6 and goes out the gluey hole on the bed die, and the aperture is 5mm, and the hole interval is 50mm, goes out gluey hole and is located bed die one side, beats a gluey hole of advancing in the middle of the bed die one side, and the aperture is 5mm, and metal injection mould material is the steel.
The solvent-free liquid polycarbosilane precursor is used as injection resin, the solvent-free liquid polycarbosilane precursor is milky transparent liquid at normal temperature, has no solvent and has viscosity of 40mPa & s at 25 ℃, and is provided by national defense science and technology university.
Before use, the solvent-free liquid polycarbosilane is put into a glue injection tank, and vacuum defoamation is carried out for 1h, wherein the vacuum degree is 0.095MPa during vacuum defoamation.
Flatly placing the pre-shaped SiC/SiC arc-shaped part fiber preform in a metal injection mold cavity, plugging a proper amount of putty strips at the edge of an end head, installing silica gel strips, and assembling a mold; connecting a glue inlet of the metal injection mould with a glue outlet of the glue injection tank, and connecting the glue outlet of the metal injection mould with a vacuum system; vacuumizing, and checking the vacuum degree of the metal injection mold, wherein the vacuum degree is required to be maintained at 0.090MPa for 20 min.
Injecting resin for 40min in vacuum state, and introducing compressed gas with pressure of 0.05MPa for injection; closing all the glue outlet valves after the glue outlet of the glue outlet is stable, wherein the glue holding time is 20 min; gradually increasing the injection pressure at a speed of 0.05MPa every 30min, completely closing the valves after all the glue outlets discharge glue, and keeping the pressure for 30 min; the highest injection pressure is 0.40 MPa.
And after the injection is finished, putting the fiber preform and the metal injection mold into an oven for curing at the curing temperature of 350 ℃ for 4 h. After curing is complete, the metal injection mold is cooled with the oven.
And opening the die when the temperature of the metal injection die is reduced to 35 ℃, and taking out the cured SiC/SiC arc-shaped finished piece.
The average thickness of the cured SiC/SiC arc-shaped workpiece blank is 5.10mm, the deviation of the thickness of the cured SiC/SiC arc-shaped workpiece blank is 2.0 percent of the target size, and the cured SiC/SiC arc-shaped workpiece blank is transferred to a graphite cracking die with holes and fixed well.
And putting the cured SiC/SiC arc-shaped workpiece blank together with the graphite cracking mould with the holes into a high-temperature furnace at 800-1600 ℃ for cracking, wherein the cracking temperature is 900 ℃, the heat preservation time is 2 hours, and the pressure is normal pressure.
And after cracking, taking the SiC/SiC arc-shaped part blank together with the perforated graphite cracking mould out of a high-temperature furnace at 800-1600 ℃, putting the SiC/SiC arc-shaped part blank into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and impregnating the container at a vacuum degree of-0.1 MPa for 8 hours, and taking out the container and cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the perforated graphite cracking mould.
Putting the SiC/SiC arc-shaped part blank together with the perforated graphite cracking mould into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 3 times, taking the SiC/SiC arc-shaped part blank out of the perforated graphite cracking mould, putting the SiC/SiC arc-shaped part blank into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and dipping for 0.1MPa of vacuum degree and keeping the vacuum degree for 10 hours, taking out the SiC/SiC arc-shaped part blank, cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the SiC/SiC arc-shaped part blank, putting the SiC/SiC arc-shaped part blank into the perforated graphite cracking mould, putting the SiC/SiC arc-shaped part blank together with the perforated graphite cracking mould into the high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 9 times, increasing the weight of the SiC/SiC arc-shaped part by 1.20 percent after, and finishing the densification cycle molding of the SiC/SiC arc-shaped workpiece.
And taking the SiC/SiC arc-shaped workpiece out of the graphite cracking die with the hole, wherein the average thickness of the taken SiC/SiC arc-shaped workpiece is 5.21mm and is 4.2% thicker than the target size. And finishing the molding of the SiC/SiC arc-shaped workpiece.
The above description is only for the preferred embodiment of the present invention, and the technical solution of the present invention is not limited thereto, and any known modifications made by those skilled in the art based on the main technical idea of the present invention belong to the technical scope of the present invention, and the specific protection scope of the present invention is subject to the description of the claims.
Claims (4)
1. A molding method of a fiber reinforced SiC-based composite material is characterized by comprising the following steps:
step one, performing a fiber preform; preparing a fiber preform by taking ceramic fibers as a raw material, and ensuring that the volume fraction of the ceramic fibers is 40-50%; placing the fiber preform in a graphite mold, and performing the fiber preform by using a hot press; wherein, the mode of adopting the hot press to the pre-setting of fibre preform is: laying the fiber preform in a graphite mold, heating the hot press to 100-300 ℃, keeping the temperature for 0.5-1 h, then placing the graphite mold in the middle of a working area of the hot press, pressurizing, keeping the pressure at 1-2 MPa, preserving the heat for 2-10 h, and cooling to room temperature;
step two, the fiber reinforced SiC-based composite material is molded in a first period; packaging the fiber preform into a metal injection mold, adopting a solvent-free liquid polycarbosilane precursor as injection resin, performing vacuum and pressure injection at the pressure speed of 0.05-0.10 MPa/10-60 min to 0.20-0.40 MPa, placing the fiber preform and the metal injection mold in an oven for curing after the injection is finished, taking out the fiber reinforced SiC-based composite material blank from the metal injection mold after the curing is finished, and transferring the fiber reinforced SiC-based composite material blank into a graphite cracking mold with holes;
step three, performing densification cycle molding on the fiber reinforced SiC-based composite material; placing the fiber reinforced SiC-based composite material blank formed in the first period and a graphite cracking mold with holes into a high-temperature furnace at 800-1600 ℃ for cracking, preserving the heat for 1-2h, and cooling to room temperature; then, putting the fiber reinforced SiC-based composite material blank and a graphite cracking mould with holes into a closed container containing a solvent-free liquid polycarbosilane precursor, vacuumizing and dipping, keeping the vacuum degree at 0.1 +/-0.01 MPa for 6-12 h, taking out, cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the graphite cracking mould with holes, putting the fiber reinforced SiC-based composite material blank and the graphite cracking mould with holes into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 3-5 times, taking out the fiber reinforced SiC-based composite material blank from the graphite cracking mould with holes, putting the blank into the closed container containing the solvent-free liquid polycarbosilane precursor, vacuumizing and dipping, keeping the vacuum degree at 0.1 +/-0.01 MPa for 6-12 h, taking out, cleaning the residual solvent-free liquid polycarbosilane precursor on the surface of the fiber reinforced SiC-based composite material blank, placing the fiber reinforced SiC-based composite material blank into a graphite cracking die with holes, placing the fiber reinforced SiC-based composite material blank and the graphite cracking die with the holes into a high-temperature furnace at 800-1600 ℃ for cracking again, repeating the dipping-cracking process for 5-10 times until the weight of the cracked fiber reinforced SiC-based composite material blank is increased by less than 2%, and completing the densification cycle molding of the fiber reinforced SiC-based composite material;
the fiber reinforced SiC-based composite material part prepared by the molding method of the fiber reinforced SiC-based composite material realizes net size molding, and the thickness of the fiber preform, the solidified blank and the densified blank of the fiber reinforced SiC-based composite material is increased by no more than 5 percent.
2. The method for forming the fiber reinforced SiC-based composite material according to claim 1, wherein the graphite cracking mold with holes has a hole diameter of 1-10 mm, a hole pitch of 5-20 mm, and holes are uniformly distributed, and the graphite material is high-strength graphite.
3. The method for molding the fiber reinforced SiC-based composite material according to claim 1, wherein the metal injection mold body for the first cycle molding of the fiber reinforced SiC-based composite material comprises a female mold, a male mold and a cushion frame, and comprises a mold frame and a mold base besides the mold body; punching glue holes on the female die, wherein the hole diameter is 2-6 mm, the hole interval is 30-50 mm, punching glue holes on one side of the male die, the hole diameter is 2-6 mm, and the metal injection die is made of steel; the solvent-free liquid polycarbosilane precursor is used as injection resin, and the viscosity of the solvent-free liquid polycarbosilane precursor is 20-200 mPa & s at 25 ℃.
4. The method for forming a fiber-reinforced SiC-based composite material according to claim 1, wherein the first cycle forming method of the fiber-reinforced SiC-based composite material is,
1) flatly placing the fiber preform in a metal injection mold cavity, plugging a proper amount of putty strips at the edge of an end head, installing silica gel strips, and assembling a mold; connecting a glue inlet of the metal injection mould with a glue outlet of the glue injection tank, and connecting the glue outlet of the metal injection mould with a vacuum system; vacuumizing, and checking the vacuum degree of the mold, wherein the vacuum degree is required to be kept above 0.080MPa for 20 min; degassing the resin in vacuum, wherein the vacuum pressure difference is not lower than 0.080MPa, the degassing time is 30-60 min, and the resin is injected for 10-60 min in a vacuum state; connecting compressed gas, keeping the pressure at 0.05 + -0.01 MPa, and injecting; closing all glue outlet valves after the glue outlet of the glue outlet is stable, and keeping the pressure for 10-60 min; gradually increasing the injection pressure at a speed of 0.05-0.10 MPa every 10-60 min, and after all glue outlets discharge glue, completely closing the valves and keeping the pressure for 10-60 min; the highest pressure is not more than 0.40 MPa;
2) after injection, putting the fiber preform and the metal injection mold into an oven for curing at the curing temperature of 200-400 ℃ for 2-4 h, and after curing, cooling the metal injection mold along with the oven;
3) and (3) cooling the temperature of the metal injection mold to below 40 ℃, opening the mold, taking out the cured fiber reinforced SiC-based composite material blank, and transferring the blank into a graphite cracking mold with holes for fixing.
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| CN108218453B (en) * | 2017-12-01 | 2021-03-26 | 中国航空工业集团公司基础技术研究院 | Forming method of thin-wall conical cylindrical ceramic matrix composite component |
| CN108424162B (en) * | 2018-04-03 | 2021-03-23 | 西北工业大学 | Preparation method of ultrahigh-temperature ceramic selective modified carbon/carbon composite material |
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| CN109514696B (en) * | 2018-11-23 | 2020-05-08 | 航天特种材料及工艺技术研究所 | Deformation control method for preformed composite material forming process and application of control method |
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