CN113307643B - SiC based on one-way belt f Preparation method of/SiC composite material - Google Patents
SiC based on one-way belt f Preparation method of/SiC composite material Download PDFInfo
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Abstract
The invention relates to aBased on single-direction belt SiC f A preparation method of a/SiC composite material. Firstly, preparing a prepreg with an interface layer from a unidirectional SiC fiber belt, and preparing a plurality of layers of unidirectional SiC fiber prepreg into SiC by a hot-pressing shaping method f Preparing compact SiC by high-temperature infiltration of a/SiC-C porous molded body f A/SiC composite material. According to the invention, the hot melt yarn-unidirectional SiC fiber belt is adopted to carry out prepreg-infiltration process research, so that fiber damage caused by curling of SiC fibers in the preform weaving process is avoided; the problem that fibers are loose and difficult to form due to pyrolysis of hot melt yarns is solved by preparing the special pre-dipping slurry component; compared with the traditional plain cloth laying layer, the composite material prepared by the method has lower fiber content under the same thickness, reduces the preparation cost of the composite material, and has an engineering application prospect.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a unidirectional tape SiC-based material f A preparation method of a/SiC composite material.
Background
SiC f the/SiC composite material is taken as a typical representative of the ceramic matrix composite material, has excellent performances of high strength, high modulus, low density, high temperature oxidation resistance and the like, and is one of potential application materials of hot end components in the aerospace field. SiC preparation by infiltration process (MI) compared to precursor immersion cracking (PIP) and chemical vapor deposition (CVI) f the/SiC composite material has the characteristics of low cost, short period, high density, low porosity and the like. The prepreg-infiltration process is a novel process developed based on the infiltration process, and the process comprises the steps of preparing an interface layer by single-tow SiC fibers through a continuous tow interface deposition furnace, hanging slurry through a prepreg trough, and carrying out a wet rolling winding methodPreparing unidirectional SiC fiber tape of prepreg, and laminating and hot-pressing to form SiC f And finally, densifying the porous blank of the/SiC composite material by melting and siliconizing. Because the composite material is formed by layering the unidirectional fiber bands, the fibers do not have the problems of curling, bending and the like, so that the mechanical property of the composite material in the fiber direction is excellent. In recent years, china has started to develop relevant researches on the preparation of ceramic matrix composite materials by a prepreg-infiltration process. Patent 201810268751.X introduces SiC based on prepreg SiC fiber two-dimensional cloth f Infiltration preparation technology of/SiC composite material. The method takes SiC fiber as a reinforcement, firstly an interface layer is prepared on the surface of two-dimensional SiC fiber cloth, then the sizing of a preform is carried out by a PCS precursor impregnation pyrolysis method, and the densification of the material is realized by a method of melting and siliconizing, so that the SiC is prepared f a/SiC composite material. The patent 201910663654.5 and the patent 201910618382.7 both introduce a prepreg-infiltration-based technology, and the method comprises the steps of coating slurry on SiC fiber two-dimensional cloth, airing at normal temperature to obtain fiber prepreg, and preparing the SiCf/SiC composite material through layering, hot pressing, carbonization and infiltration.
It can be found that the current mainstream research direction is to research subsequent steps in the prepreg-infiltration process, such as layer formation, infiltration and the like, by using the SiC fiber two-dimensional cloth. This is because the prior art and equipment are in a blank state and cannot deposit an interface layer and prepare a unidirectional tape for continuous SiC monofilament tow fibers. The mechanical property of the SiC fiber can be lost due to the crossed winding of the fibers in the warp direction and the weft direction of the SiC fiber two-dimensional cloth, and the performance of the final composite material is influenced; meanwhile, the cross nodes of the warp and weft fibers are easy to generate the defects of pores and the like, and the overall density of the composite material is influenced. It is a necessary trend to investigate prepreg-infiltration processes based on unidirectional SiC fiber tapes.
Therefore, the inventor provides a unidirectional tape SiC-based material f A preparation method of a/SiC composite material.
Disclosure of Invention
(1) Technical problem to be solved
The embodiment of the invention provides a unidirectional tape SiC-based material f Preparation method of/SiC composite materialThe method solves the problems that the SiCf/SiC composite material prepared by the prior art has poor mechanical property in the fiber direction due to fiber damage caused by curling in the process of weaving a preform, and the overall compactness of the composite material is influenced due to the defects that the positions of cross nodes of warp and weft fibers are easy to generate holes and the like.
(2) Technical scheme
The embodiment of the invention provides a unidirectional tape SiC-based material f The preparation method of the/SiC composite material comprises the following steps S110 to S160:
step S110, preparing an interface phase: and clamping the single-layer hot-melt yarn-unidirectional SiC fiber belt by using a mold, and putting the single-layer hot-melt yarn-unidirectional SiC fiber belt into an interface layer deposition furnace to prepare a boron nitride interface phase.
Step S120, preparing a prepreg slurry: preparing the prepreg slurry by using SiC powder, an organic carbon source and an organic solvent according to the ratio of 3.
Step S130, preparing a unidirectional SiC fiber prepreg: and (2) putting the unidirectional SiC fiber tape containing the boron nitride interface phase with the die in the step (S110) into a vacuum container for dipping, firstly vacuumizing, then filling the prepreg slurry prepared in the step (S120), maintaining the pressure for 4-12 h, then taking out, putting into an oven for drying, and demolding to obtain the unidirectional SiC fiber prepreg.
Step S140, laminating and hot-press molding: and (4) coating adhesives on two surfaces of the 5-20 layers of unidirectional SiC fiber prepreg tapes obtained in the step (S130), laying the unidirectional SiC fiber prepreg tapes in the direction of fiber cloth, and curing and molding the unidirectional SiC fiber prepreg tapes by a hot pressing process to obtain a porous molded body.
Step S150, pyrolysis: putting the porous formed body obtained in the step S140 into a high-temperature cracking furnace for cracking, and naturally cooling to obtain SiC f A SiC-C porous body.
Step S160, high-temperature infiltration: siC obtained in step S150 f Putting the/SiC-C porous body into an infiltration furnace, embedding Si powder for high-temperature infiltration, and naturally cooling to obtain compact SiC f a/SiC composite material.
Further, in step S110, the thermal melting yarn-unidirectional SiC fiber tape is woven in a plain weave with SiC fibers in the warp direction and thermal melting yarns in the weft direction.
Further, in the step S110, the thickness of the boron nitride interphase is 100nm to 500nm.
Further, in the step S120, the organic carbon source is at least one of furan resin, furfuryl ketone resin, and phenolic resin, and the organic solvent is ethanol or acetone.
Further, in step S130, the conditions for placing into an oven to dry are as follows: heating to 160-240 ℃, and keeping the temperature for 2-24 h.
Further, in step S140, the adhesive is one of furan resin, phenolic resin, and liquid polycarbosilane.
Further, in step S140, the conditions for curing and molding through the hot pressing process are as follows: heating from room temperature to 160-240 ℃ at a heating rate of 5-10 ℃/min, keeping the temperature at 2-4 MPa for 0.5-2 h.
Further, in step S150, the cracking conditions in the pyrolysis furnace are as follows: heating from room temperature to 800-1200 ℃ at a heating rate of 100-600 ℃/h, keeping the temperature for 0.5-2 h, and keeping the pressure in vacuum.
Further, in step S150, the conditions for performing high-temperature infiltration in the infiltration furnace are as follows: heating from room temperature to 1410-1500 ℃ at a heating rate of 100-600 ℃/h, keeping the temperature for 1-4 hours, and keeping the pressure in vacuum.
(3) Advantageous effects
Firstly, the invention utilizes the characteristic of high-temperature decomposition of the hot melt yarn, the hot melt yarn can be completely decomposed in the deposition and heating process of the interface layer of the composite material, the subsequent process is not influenced, and impurities are not introduced, so that the SiC fiber is unidirectionally retained in the composite material, and the effect of using the unidirectional SiC fiber band as a reinforcement is achieved.
Secondly, after the hot melt yarn-unidirectional SiC fiber belt is used for preparing the interface layer, the hot melt yarn is decomposed, and the unidirectional SiC fibers do not have binding force and can be dispersed, so that the subsequent forming process is influenced. According to the invention, through designing the special slurry component, the dispersed SiC fibers can be fixed through the slurry matrix after the prepreg is prepared, and the fibers are not loose after demolding, so that the feasibility of a subsequent hot-press molding process is ensured.
Finally, compared with the traditional SiC fiber two-dimensional cloth, the composite material prepared based on the hot melt yarn-unidirectional SiC fiber tape has lower fiber volume fraction, and the SiC is reduced f Preparation cost of/SiC composite material, siC prepared by the method of the invention f the/SiC composite material has better mechanical property and integral compactness.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 shows a unidirectional tape-based SiC device according to an embodiment of the present invention f A process flow chart of a preparation method of the/SiC composite material.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are provided to illustrate the principles of the invention and are not intended to limit the scope of the invention, i.e., the invention is not limited to the embodiments described, but covers any modification, replacement, or improvement of the devices and modes of operation without departing from the spirit of the invention.
It should be noted that, in the present application, the embodiments and features of the embodiments may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Example 1
Referring to fig. 1, the invention provides a preparation method of a composite material based on SiCf/SiC with a unidirectional tape, which includes the following steps S110 to S160:
step S110, preparing an interface phase: clamping a single-layer hot-melt yarn-unidirectional SiC fiber band by using a mold, and putting the single-layer hot-melt yarn-unidirectional SiC fiber band into an interface layer deposition furnace to prepare a Boron Nitride (BN) interface phase, wherein the thickness of the boron nitride interface phase is 200nm.
In the step, the thermal melting yarn-unidirectional SiC fiber tape adopts domestic SiC fiber in the warp direction, the thermal melting yarn in the weft direction and the fabric weave is plain weave.
Step S120, preparing a prepreg slurry: preparing prepreg slurry by using 30 parts of SiC powder, 50 parts of organic carbon source and 20 parts of organic solvent, and performing ball milling for 24 hours to obtain uniformly mixed prepreg slurry. In this example, furan resin was used as the organic carbon source, and acetone was used as the organic solvent.
Step S130, preparing unidirectional SiC fiber prepreg: and (2) putting the unidirectional SiC fiber tape containing the boron nitride interface phase with the die in the step (S110) into a vacuum container for dipping, firstly vacuumizing, then filling the prepreg slurry prepared in the step (S120), maintaining the pressure for 10h, then taking out, putting into an oven, heating to 200 ℃, preserving the heat for 4h, drying, and demolding to obtain the unidirectional SiC fiber prepreg.
Step S140, laminating and hot-press molding: and (2) coating adhesives on two surfaces of 10 layers of the unidirectional SiC fiber prepreg tapes obtained in the step S130, sequentially laying according to the direction of fiber cloth [ 0-90-0-90 degrees ] (namely, according to the fact that the first layer of fiber tape is transversely laid along the length, the next layer of fiber tape is longitudinally laid along the length, and the two adjacent layers of fiber tapes are crossly laid), heating to 200 ℃ from room temperature at the heating rate of 10 ℃/min, keeping the temperature at 3MPa, keeping the temperature for 2 hours, and carrying out curing molding through a hot pressing process to obtain a porous molded body. The binder in this example is furan resin.
Step S150, pyrolysis: putting the porous formed body obtained in the step S140 into a high-temperature cracking furnace for vacuum cracking, heating the porous formed body from room temperature to 1200 ℃ at the heating rate of 300 ℃/h, preserving the heat for 1h, and naturally cooling to obtain SiC f An SiC-C porous body.
Step S160, high-temperature infiltration: siC obtained in step S150 f Putting the/SiC-C porous body into an infiltration furnace, embedding the porous body by using Si powder, heating the porous body from room temperature to 1450 ℃ at the heating rate of 300 ℃/h, preserving the heat for 2 hours under the vacuum pressure, carrying out high-temperature infiltration, and naturally cooling to obtain compact SiC f Composite of/SiCA material.
After testing, the prepared SiC f The density of the/SiC composite material is 2.65g/cm 3 Porosity was 3.9%, and tensile strength in the 0 ℃ direction was 283MPa.
Example 2
Step S110, preparing an interface phase: clamping a single-layer hot-melt yarn-unidirectional SiC fiber band by using a mold, and putting the single-layer hot-melt yarn-unidirectional SiC fiber band into an interface layer deposition furnace to prepare a Boron Nitride (BN) interface phase, wherein the thickness of the boron nitride interface phase is 200nm.
In the step, the thermal melting yarn-unidirectional SiC fiber tape adopts domestic SiC fiber in the warp direction, the thermal melting yarn in the weft direction and the fabric weave is plain weave.
Step S120, preparing prepreg slurry: preparing prepreg slurry by using 30 parts of SiC powder, 50 parts of organic carbon source and 20 parts of organic solvent, and performing ball milling for 24 hours to obtain uniformly mixed prepreg slurry. In this example, furan resin was used as the organic carbon source, and acetone was used as the organic solvent.
Step S130, preparing unidirectional SiC fiber prepreg: and (2) putting the unidirectional SiC fiber tape containing the boron nitride interface phase with the die in the step (S110) into a vacuum container for dipping, firstly vacuumizing, then filling the prepreg slurry prepared in the step (S120), maintaining the pressure for 10h, then taking out, putting into an oven, heating to 200 ℃, preserving the heat for 4h, drying, and demolding to obtain the unidirectional SiC fiber prepreg.
Step S140, laminating and hot-press molding: coating adhesive on two surfaces of 10 layers of the unidirectional SiC fiber prepreg tapes obtained in the step S130, sequentially laying according to the direction [ 0-90-0-90 degrees ] of fiber cloth (namely, transversely laying the first two layers of fiber tapes along the length, longitudinally laying the next layer of fiber tapes along the length, transversely laying the second two layers of fiber tapes along the length, and laying the adjacent two layers of fiber tapes in the cross direction), heating from room temperature to 200 ℃ at the heating rate of 10 ℃/min, keeping the temperature at 3MPa, preserving the heat for 2 hours, and curing and forming through a hot pressing process to obtain a porous formed body. The adhesive in this embodiment is furan resin.
Step S150, pyrolysis: putting the porous formed body obtained in the step S140 into a high-temperature cracking furnace for vacuum cracking, and raising the temperature at 300 ℃/hHeating the mixture from room temperature to 1200 ℃, preserving the heat for 1 hour, and naturally cooling to obtain SiC f An SiC-C porous body.
Step S160, high-temperature infiltration: siC obtained in step S150 f Putting the/SiC-C porous body into an infiltration furnace, embedding the porous body by using Si powder, heating the porous body from room temperature to 1450 ℃ at the heating rate of 300 ℃/h, preserving the heat for 2 hours under the vacuum pressure, carrying out high-temperature infiltration, and naturally cooling to obtain compact SiC f a/SiC composite material.
After testing, the prepared SiC f The density of the/SiC composite material is 2.68g/cm 3 The porosity was 3.2%, and the tensile strength in the 0 ℃ direction was 311MPa.
The appearance quality and the internal quality of the molded composite material blade 10 are detected, and both the appearance quality and the internal quality meet the design requirements.
The above description is only an example of the present application and is not limited to the present application. Various modifications and alterations to this application will become apparent to those skilled in the art without departing from the scope of this invention. Any modification, equivalent replacement, improvement or the like made within the spirit and principle of the present application shall be included in the scope of the claims of the present application.
Claims (1)
1. SiC based on one-way belt f The preparation method of the/SiC composite material is characterized by comprising the following steps:
step S110, preparing an interface phase: clamping the single-layer hot-melt yarn-unidirectional SiC fiber belt by using a mold, and putting the single-layer hot-melt yarn-unidirectional SiC fiber belt into an interface layer deposition furnace to prepare a boron nitride interface phase; the warp direction of the hot melt yarn-unidirectional SiC fiber tape is SiC fiber, the weft direction of the hot melt yarn-unidirectional SiC fiber tape is hot melt yarn, and the fabric weave is plain weave; the thickness of the boron nitride interface phase is 100 nm-500 nm;
step S120, preparing a prepreg slurry: preparing prepreg slurry by using SiC powder, an organic carbon source and an organic solvent according to the proportion of 3; the organic carbon source is at least one of furan resin, furfuryl ketone resin and phenolic resin, and the organic solvent is ethanol or acetone;
step S130, preparing unidirectional SiC fiber prepreg: putting the unidirectional SiC fiber tape containing the boron nitride interface phase with the die in the step S110 into a vacuum container for dipping, firstly vacuumizing, then pouring the prepreg slurry prepared in the step S120, maintaining the pressure for 4-12 h, then taking out, putting into an oven for drying, and demoulding to obtain unidirectional SiC fiber prepreg; the conditions of drying in an oven are as follows: heating to 160-240 ℃, and keeping the temperature for 2-24 h;
step S140, laminating and hot-press molding: coating adhesives on two surfaces of the 5-20 layers of unidirectional SiC fiber prepreg tapes obtained in the step S130, laying the unidirectional SiC fiber prepreg tapes in the direction of fiber cloth, and curing and forming through a hot pressing process to obtain a porous formed body; the adhesive is one of furan resin, phenolic resin and liquid polycarbosilane; the conditions for curing and molding by the hot pressing process are as follows: heating from room temperature to 160-240 ℃ at a heating rate of 5-10 ℃/min, keeping the pressure at 2-4 MPa, and keeping the temperature for 0.5-2 hours;
step S150, pyrolysis: putting the porous formed body obtained in the step S140 into a high-temperature cracking furnace for cracking, and naturally cooling to obtain SiC f A SiC-C porous body; the conditions for cracking in the pyrolysis furnace are as follows: heating from room temperature to 800-1200 ℃ at a heating rate of 100-600 ℃/h, keeping the temperature for 0.5-2 h, and keeping the pressure in vacuum;
step S160, high-temperature infiltration: siC obtained in step S150 f Putting the/SiC-C porous body into an infiltration furnace, embedding Si powder for high-temperature infiltration, and naturally cooling to obtain compact SiC f a/SiC composite material; the conditions for high-temperature infiltration in the infiltration furnace are as follows: heating from room temperature to 1410-1500 deg.c at the heating rate of 100-600 deg.c/h, maintaining for 1-4 hr and vacuum pressure.
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| CN116444286A (en) * | 2023-01-30 | 2023-07-18 | 合肥富维康新材料科技有限公司 | Method for improving melt siliconizing uniformity of MI-SiC-SiC preform |
| CN116354737A (en) * | 2023-04-03 | 2023-06-30 | 合肥富维康新材料有限公司 | Method for precisely controlling volume fraction of SiC fibers in MI-SiC/SiC composite material |
| CN116375487A (en) * | 2023-04-03 | 2023-07-04 | 合肥富维康新材料有限公司 | Preparation method of low-porosity SiC fiber unidirectional prepreg tape |
| CN116396088A (en) * | 2023-04-03 | 2023-07-07 | 合肥富维康新材料有限公司 | Method for improving melt siliconizing uniformity of MI-SiC/SiC preform and interlayer binding force of composite material |
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