CN111943726B - High-performance C/SiBCN composite material and preparation method and application thereof - Google Patents
High-performance C/SiBCN composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a high-performance C/SiBCN composite material and a preparation method and application thereof. The method comprises the following steps: preparing a C interface layer and a SiC interface layer on the surface of the carbon fiber preform and/or alternately depositing the C interface layer and the SiC interface layer (C/SiC) n Alternating interface layers to obtain a modified carbon fiber preform; and (3) taking a liquid SiBCN precursor as an impregnation liquid, and performing SiBCN matrix densification on the modified carbon fiber preform by a PIP (Poly-p-phenylene-diisocyanate) process of vacuum impregnation/in-situ curing/medium-pressure cracking to obtain the high-performance C/SiBCN composite material. The invention prepares a proper interface layer, and realizes the toughening function; the invention adopts the in-situ curing process, avoids the outflow of the precursor in the curing process, improves the impregnation depth and the impregnation efficiency, and simultaneously adopts the medium-pressure cracking process, reduces SiBCN matrix cracks, reduces the porosity of the material and improves the mechanical property of the composite material.
Description
Technical Field
The invention belongs to the technical field of thermostructural composite materials, and particularly relates to a high-performance C/SiBCN composite material as well as a preparation method and application thereof.
Background
The C/SiBCN ceramic matrix composite material has the advantages of low density, high temperature resistance, high specific modulus,High specific strength, oxidation resistance and other excellent performances, and has wide application prospect in the field of aerospace. The quaternary SiBCN amorphous ceramic matrix generates BN/B in the ceramic conversion process by introducing boron 4 Phase C, BN/B 4 The C phase has good high-temperature thermal stability, the crystallization temperature of the material is increased, the high-temperature resistance of the ceramic matrix is greatly improved, and the normal-temperature and high-temperature mechanical properties and the oxidation resistance of the ceramic matrix are excellent.
PIP process (precursor impregnation cracking process) is the main preparation process for preparing C/SiBCN composite materials. The PIP technology is that polyborosilazane solution is dipped into a porous carbon fiber prefabricated body under a certain vacuum degree, then pressure dipping and pressure curing are carried out, and finally the polyborosilazane is cracked at a certain temperature to obtain a SiBCN matrix, thereby preparing the C/SiBCN composite material. Lee and the like adopt boron-containing micromolecular compounds and low-viscosity polysilazane to blend as SiBCN ceramic precursors, and adopt a PIP method to prepare the C/SiBCN ceramic matrix composite material, wherein the room-temperature bending strength of the composite material is 255MPa (see: liuwei, caocamei, wanling, et al. RTM forming process for C/SiBCN ceramic matrix composite material f Effect of/SiBCN ceramic matrix composite Properties [ J]Material engineering, 2015,43 (006): 1-6.). The C/SiBCN ceramic matrix composite material is prepared by poly-boron silazane (P-SiBCN) serving as a precursor and a PIP process, and the room-temperature bending strength of the C/SiBCN ceramic matrix composite material reaches 334MPa (see: wangxujun, zhang Zongbo, zengfan, and the like]Aerospace materials technology, 2013,43 (2): 47-50.). The Chinese patent application CN104591768A adopts a SiBCN precursor modified by using the silicon alkyne and adopts a PIP process to prepare the C/SiBCN composite material, and the room-temperature bending strength can only reach 374MPa.
In summary, the mechanical properties of the existing C/SiBCN composite material are relatively low and need to be further improved. Therefore, it is very necessary to provide a high-performance C/SiBCN composite material with excellent mechanical properties and a preparation method thereof.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a high-performance C/SiBCN composite material and a preparation method and application thereof.
The invention provides a preparation method of a high-performance C/SiBCN composite material in a first aspect, which comprises the following steps:
(1) Preparing a C interface layer and a SiC interface layer on the surface of the carbon fiber preform and/or alternately depositing the C interface layer and the SiC interface layer (C/SiC) n Alternating interface layers to obtain a modified carbon fiber preform;
(2) And carrying out SiBCN matrix densification on the modified carbon fiber preform by taking a liquid SiBCN precursor as an impregnation liquid through a PIP (Poly ethylene propylene) process of vacuum impregnation/in-situ curing/medium-pressure cracking to obtain the high-performance C/SiBCN composite material.
Preferably, the PIP process of vacuum impregnation/in situ curing/medium pressure cracking comprises the following sub-steps:
(a) Placing the modified carbon fiber preform in a vacuum bag, and taking the liquid SiBCN precursor as an impregnation liquid for vacuum impregnation;
(b) Putting the vacuum bag filled with the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor into a curing tank to carry out in-situ curing on the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor, thereby obtaining a carbon fiber composite material;
(c) And taking the carbon fiber composite material out of the vacuum bag, and then placing the carbon fiber composite material in a medium-pressure cracking furnace for high-temperature medium-pressure cracking.
Preferably, the vacuum impregnation time is 1.5-3 h; and/or the temperature of the in-situ curing is 180-280 ℃, and the time of the in-situ curing is 3-6 h; and/or carrying out high-temperature medium-pressure cracking in a nitrogen atmosphere or an argon atmosphere, wherein the temperature of the high-temperature medium-pressure cracking is 800-1100 ℃, the pressure of the high-temperature medium-pressure cracking is 2-6 MPa, and the time of the high-temperature medium-pressure cracking is 2-7 h.
Preferably, step (2) is repeated 4 to 6 times.
Preferably, in said (C/SiC) n N =1 to 3 in the alternating interface layers.
Preferably, the density of the modified carbon fiber preform is 0.2 to 0.80g/cm 3 。
Preferably, the viscosity of the liquid SiBCN precursor is less than 20mPa · s.
Preferably, the density of the high-performance C/SiBCN composite material is not less than 1.9g/cm 3 The room temperature bending strength is not lower than 700MPa, the bending strength under the air atmosphere of 1000 ℃ is not lower than 500MPa, and the bending strength under the inert atmosphere of 1400 ℃ is not lower than 650MPa.
In a second aspect, the present invention provides a high performance C/SiBCN composite material prepared by the preparation method of the first aspect of the invention.
In a third aspect, the present invention provides the use of the high performance C/SiBCN composite material obtained by the preparation method according to the first aspect of the present invention as a thermostructural composite material.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) In some more preferred embodiments, a typical composite material (X/Y) n interface layer structure is realized through an alternative structure design of PyC and SiC, and when cracks are expanded to the composite interface layer, the cracks are subjected to turning propagation among sub-layers to realize the toughening function of the composite material, so that the mechanical property of the composite material is improved.
(2) The method adopts the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking to densify the SiBCN matrix, adopts the in-situ curing process, avoids the outflow of a liquid SiBCN precursor in the curing process, improves the impregnation depth and the impregnation efficiency, simultaneously adopts the medium-pressure cracking process, reduces the SiBCN matrix cracks, obviously reduces the porosity of the composite material, and improves the mechanical property of the composite material.
(3) The density of the high performance C/SiBCN composite material prepared in some preferred embodiments of the present invention is not less than 1.9g/cm 3 The room temperature bending strength is not lower than 700MPa, the bending strength under the air atmosphere of 1000 ℃ is not lower than 500MPa, the bending strength under the inert atmosphere of 1400 ℃ is not lower than 650MPa, and the mechanical property of the composite material is far better than that of the existing C/SiBCN composite material.
Drawings
FIG. 1 is a micro-topography (SEM image) of a high performance C/SiBCN composite made in example 3 of the present invention.
FIG. 2 is a stress-strain curve of the C/SiBCN composite prepared in example 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It should be apparent that the described embodiments are only some of the embodiments of the present invention, and not all of them. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The invention provides a preparation method of a high-performance C/SiBCN composite material in a first aspect, which comprises the following steps:
(1) Preparing a C interface layer and a SiC interface layer on the surface of the carbon fiber preform and/or alternately depositing the C interface layer and the SiC interface layer (C/SiC) n Alternating interface layers to obtain a modified carbon fiber preform; in the invention, the carbon fiber preform can adopt a 3D structure porous carbon fiber preform such as a needle punching structure, a two-dimensional carbon cloth lamination sewing structure or fine weaving puncture; in the present invention, for example, the C interface layer, the SiC interface layer and/or the (C/SiC) layer may be prepared by a CVI process n Alternating interface layers; in the present invention, (C/SiC) n The alternating interface layers are marked as C and SiC alternating interface layers;
(2) Performing SiBCN matrix densification on the modified carbon fiber preform by using a liquid SiBCN precursor (liquid polyborosilazane) as an impregnation liquid through a PIP (precursor impregnation cracking) process of vacuum impregnation/in-situ curing/medium-pressure cracking, preferably performing multiple PIP cycles to obtain a high-performance C/SiBCN composite material; in the present invention, for example, the step (2) may be repeated a plurality of times (e.g., 4 to 6 times) to obtain the high performance C/SiBCN composite material.
According to the invention, a C interface layer, a SiC interface layer and/or a C and SiC alternative interface layer are/is prepared on the surface of carbon fiber of a carbon fiber preform, and then the high-performance C/SiBCN composite material is obtained by performing SiBCN matrix densification for multiple times by adopting a vacuum impregnation/in-situ curing/medium-pressure cracking PIP process.
As is well known, an interface layer structure is arranged in a carbon fiber composite material, when cracks extend to the interface layer, the cracks are subjected to steering propagation among sub-layers, and the toughening function of the carbon fiber composite material is realized, so that the mechanical property of the composite material can be improved, but no relevant report which clearly indicates that the interface layer is prepared on the surface of a carbon fiber preform in the conventional method for preparing the C/SiBCN composite material by using a PIP (poly-propylene-based carbon/silicon-on-carbon) process is found, which probably causes that the influence research on the interface layer is insufficient; those skilled in the art know that when a SiBCN precursor solution (polyborosilazane solution) is used for a precursor impregnation cracking process, the cured SiBCN precursor is attached to the surface of carbon fibers, and in a high-temperature cracking process, due to the release of small molecules, the precursor shrinks, thereby damaging the carbon fibers and reducing the mechanical properties of the C/SiBCN composite material prepared by a PIP process.
The method overcomes the technical bias, prepares a proper interface layer on the surface of the carbon fiber preform, and matches with an improved PIP process, namely, adopts the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking to perform SiBCN matrix densification, and the inventor finds that the in-situ curing process is adopted, so that the SiBCN precursor is prevented from flowing out in the curing process, the liquid SiBCN precursor is ensured to enter the interior of the carbon fiber preform, the impregnation depth and the impregnation efficiency are improved, and simultaneously adopts the medium-pressure cracking process, so that the SiBCN precursor cracking yield is improved, the release of small molecules is reduced, the SiBCN matrix cracks are reduced, the porosity of the composite material is obviously reduced, and the mechanical property of the composite material is improved; the invention improves the cracking yield of SiBCN precursor, reduces the damage to the fiber caused by the release of small molecules in the cracking process, prepares a proper interface layer on the surface of the carbon fiber preform for the first time, and more preferably prepares the (C/SiC) n The invention realizes a typical composite material (X/Y) n interface layer structure by the alternative structure design of PyC (C interface layer) and SiC (SiC interface layer), when cracks extend to the composite interface layer, the cracks can perform steering transmission among all sub-layersThe mechanical property of the high-performance C/SiBCN composite material prepared by the invention is obviously superior to that of the existing C/SiBCN composite material; in some more preferred embodiments of the present invention, it is ensured that a density of not less than 1.9g/cm is obtained 3 The room temperature bending strength is not lower than 700MPa, the bending strength under the air atmosphere of 1000 ℃ is not lower than 500MPa, the bending strength under the inert atmosphere of 1400 ℃ is not lower than 650MPa, and the mechanical property of the composite material is far superior to that of the existing C/SiBCN composite material.
According to some preferred embodiments, the PIP process of vacuum impregnation/in situ curing/medium pressure cracking comprises the following sub-steps:
(a) Placing the modified carbon fiber preform in a vacuum bag, and taking the liquid SiBCN precursor as an impregnation liquid for vacuum impregnation; in the invention, for example, after the modified carbon fiber preform is placed in a vacuum bag and vacuumized, a liquid SiBCN precursor is sucked for vacuum impregnation;
(b) Putting a vacuum bag filled with the modified carbon fiber preform (the vacuum-impregnated modified carbon fiber preform) vacuum-impregnated with the liquid SiBCN precursor into a curing tank to cure the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor in situ to obtain a carbon fiber composite material;
(c) Taking the carbon fiber composite material out of the vacuum bag, and then placing the carbon fiber composite material in a medium-pressure cracking furnace for high-temperature medium-pressure cracking, wherein the pressure of the high-temperature medium-pressure cracking is 3 MPa-6 MPa; in the present invention, the parameters of the vacuum impregnation in step (a) and the in-situ curing temperature and time in step (b) may be, for example, the vacuum impregnation parameters and the curing parameters related to the PIP process performed by using the existing SiBCN precursor as an impregnation solution, and those skilled in the art may set the parameters according to specific requirements.
In the invention, the modified carbon fiber preform which is not vacuum-impregnated with the liquid SiBCN precursor is taken out of a vacuum bag and is directly put into a curing tank together with the vacuum bag for in-situ curing, and after the curing is finished, the material is taken out of the vacuum bag and is put into a medium-pressure cracking furnace for high-temperature medium-pressure cracking; the PIP process is characterized in that the dipped blank body is taken out and then placed in a curing tank for curing, and then normal-pressure cracking is carried out; compared with the existing method for preparing the C/SiBCN composite material, the method adopts the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking to densify the SiBCN matrix, adopts the in-situ curing process, avoids the outflow of a liquid SiBCN precursor in the curing process, improves the impregnation depth and the impregnation efficiency, and simultaneously adopts the medium-pressure cracking process to improve the cracking yield of the SiBCN precursor, reduce the emission of small molecules, reduce the cracks of the SiBCN matrix, obviously reduce the porosity of the composite material and obviously improve the mechanical property of the composite material.
According to some preferred embodiments, the vacuum impregnation is for a time of 1.5 to 3 hours (e.g. 1.5, 2, 2.5 or 3 hours); and/or the temperature of the in situ cure is 180 to 280 ℃ (e.g., 180 ℃, 190 ℃, 200 ℃, 210 ℃, 220 ℃, 230 ℃, 240 ℃, 250 ℃, 260 ℃, 270 ℃ or 280 ℃), and the time of the in situ cure is 3 to 6 hours (e.g., 3, 3.5, 4, 4.5, 5, 5.5 or 6 hours); and/or the high-temperature medium-pressure cracking is carried out in a nitrogen atmosphere or an argon atmosphere, the temperature of the high-temperature medium-pressure cracking is 800-1100 ℃ (such as 800 ℃, 850 ℃, 900 ℃, 950 ℃,1000 ℃, 1050 ℃ or 1100 ℃), the pressure of the high-temperature medium-pressure cracking is 3-6 MPa (such as 3MPa, 4MPa, 5MPa or 6 MPa), and the time of the high-temperature medium-pressure cracking is 2-7 h (such as 2, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5 or 7 h). In the invention, the temperature of the high-temperature medium-pressure cracking is preferably 800-1100 ℃, if the temperature of the high-temperature medium-pressure cracking is too low, the SiBCN cracking can be incomplete, and the efficiency is reduced; if the high-temperature and medium-temperature cracking temperature is too high, new cracks can be generated in the composite material, and the performance of the composite material is adversely affected; in the invention, the pressure of the high-temperature medium-pressure cracking is preferably 3MPa to 6MPa, if the pressure is too low, the effect of reducing SiBCN matrix crack generation and porosity of the composite material is not obvious, and the effect of improving the performance of the composite material is not obvious; if the pressure is too high, the requirement on equipment is further increased, and the equipment cost is greatly increased.
According to some preferred embodiments, step (3) is repeated 4 to 6 times (e.g. 4, 5 or 6 times).
According to some preferred embodiments, in said (C/SiC) n N =1 to 3 (e.g., 1, 2, or 3) in the alternating interface layers; that is, in the present invention, the (C/SiC) is preferred n The alternating interface layers are C/SiC alternating interface layers, C/SiC/C/SiC alternating interface layers or C/SiC/C/SiC/C/SiC alternating interface layers.
According to some preferred embodiments, the C interface layer, the SiC interface layer and/or the (C/SiC) are prepared using a CVI process n Alternating interface layers; the deposition time is 50-100 h when preparing the C interface layer, 50-100 h when preparing the SiC interface layer, and/or the (C/SiC) n When the interface layers are alternated, the deposition time of each C interface layer is 10h, and the deposition time of each SiC interface layer is 15h; in the present invention, the C interface layer, the SiC interface layer and/or the (C/SiC) are deposited n The alternating of the interface layers can be performed, for example, by using a CVI process known in the art, and can be set by those skilled in the art according to specific requirements.
According to some preferred embodiments, the modified carbon fiber preform has a density of 0.2 to 0.80g/cm 3 。
According to some preferred embodiments, the SiBCN precursor is a liquid precursor having a viscosity < 20mPa · s; due to the low viscosity, the liquid SiBCN precursor (liquid polyborosilazane) has good wettability to the carbon fiber preform and can enter the fiber bundle, so that the porosity of the composite material is reduced, and the mechanical property of the composite material is improved.
According to some preferred embodiments, the high performance C/SiBCN composite has a density of not less than 1.9g/cm 3 The room-temperature bending strength is not less than 700MPa, the bending strength at 1000 ℃ in an air atmosphere is not less than 500MPa, and the bending strength at 1400 ℃ in an inert atmosphere (such as nitrogen or argon) is not less than 650MPa.
According to some specific embodiments, the method for preparing the high-performance C/SiBCN composite material comprises the following steps:
first, aStep, preparing an interface layer by adopting a CVI (chemical vapor infiltration) process, which specifically comprises the following steps: preparing a low-density C interface layer on the surface of a carbon fiber preform by adopting a 3D structure carbon fiber preform with a needling structure, a two-dimensional carbon cloth laminated sewing structure or a fine weaving and puncturing structure and the like and adopting a chemical vapor deposition (CVI) process, wherein the deposition time is 50-100 h; or preparing a SiC interface layer on the surface of the carbon fiber preform by adopting a CVI process, wherein the deposition time is 50-100 h; or preparing a C and SiC alternating interface layer ((C/SiC) on the surface of the carbon fiber preform by adopting a CVI (chemical vapor infiltration) process n Alternate interface layers), C deposition time 10h, siC deposition time 15h, (C/SiC) n The alternating interface layers are C/SiC, C/SiC/C/SiC or C/SiC/C/SiC/C/SiC.
Secondly, using liquid polyborosilazane as a SiBCN precursor, performing SiBCN matrix densification on the material with the interface layer prepared in the first step by adopting a PIP (Poly-p-phenylene-bis-phenyl) process of vacuum impregnation/in-situ curing/medium-pressure cracking, and performing vacuum impregnation, in-situ curing and medium-pressure cracking, wherein the PIP process is a PIP process of one-step vacuum impregnation/in-situ curing/medium-pressure cracking; the cycle times of the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking are 4-6 times, and the high-performance C/SiBCN composite material is obtained.
In a second aspect, the invention provides a high-performance C/SiBCN composite material prepared by the preparation method of the first aspect; the mechanical property of the C/SiBCN composite material prepared by the invention is obviously superior to that of the existing C/SiBCN composite material.
In a third aspect, the present invention provides the use of the high performance C/SiBCN composite material obtained by the preparation method according to the first aspect of the present invention as a thermostructural composite material.
The invention will be further illustrated by way of example, but the scope of protection is not limited to these examples.
Example 1
(1) The carbon fiber preform with a carbon cloth laminated sewing structure is adopted, and the density of the preform is 0.65-0.80 g/cm 3 And preparing a C interface layer by adopting a CVI (chemical vapor infiltration) process (CVI), and depositing for 100 hours to obtain the modified carbon fiber preform.
(2) Taking a liquid SiBCN precursor (liquid polyborosilazane) as an impregnation liquid, adopting a PIP (poly-p-phenylene) process of vacuum impregnation/in-situ curing/medium-pressure cracking to perform SiBCN matrix densification on the modified carbon fiber preform, and performing vacuum impregnation, in-situ curing and medium-pressure cracking, which is a PIP process of one-step vacuum impregnation/in-situ curing/medium-pressure cracking; the circulation frequency of the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking is 6 times, so that the high-performance C/SiBCN composite material is obtained; the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking at each time specifically comprises the following steps: placing the modified carbon fiber preform in a vacuum bag, taking the liquid SiBCN precursor as impregnation liquid for vacuum impregnation, after vacuum impregnation for 2h, placing the vacuum bag filled with the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor into a curing tank to carry out in-situ curing on the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor, wherein the in-situ curing temperature is 250 ℃, and the in-situ curing time is 4 hours, so as to obtain a carbon fiber composite material; and finally, taking the carbon fiber composite material out of the vacuum bag, and then putting the carbon fiber composite material into a medium-pressure cracking furnace to perform high-temperature medium-pressure cracking for 3 hours at the temperature of 1000 ℃ and under the pressure of 4MPa in a nitrogen atmosphere.
The density of the high-performance C/SiBCN composite material prepared by the embodiment is 1.90g/cm 3 The room-temperature bending strength was 442MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 298MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 503MPa.
Example 2
(1) The carbon fiber preform with a carbon cloth laminated sewing structure is adopted, and the density of the preform is 0.65-0.80 g/cm 3 And preparing a SiC interface layer by adopting a CVI (chemical vapor infiltration) process (CVI), and depositing for 100h to obtain the modified carbon fiber preform.
(2) The preparation method comprises the following steps of taking a liquid SiBCN precursor (liquid polyborosilazane) as an impregnation liquid, adopting a PIP (Poly-p-phenylene-bis-phenyl) process of vacuum impregnation/in-situ curing/medium-pressure cracking to perform SiBCN matrix densification on a modified carbon fiber preform, and performing vacuum impregnation, in-situ curing and medium-pressure cracking, wherein the PIP process is a PIP process of one-step vacuum impregnation/in-situ curing/medium-pressure cracking; the circulation frequency of the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking is 6 times, so that the high-performance C/SiBCN composite material is obtained; the PIP process of each vacuum impregnation/in-situ curing/medium-pressure cracking specifically comprises the following steps: placing the modified carbon fiber preform in a vacuum bag, taking the liquid SiBCN precursor as impregnation liquid for vacuum impregnation, after vacuum impregnation for 2h, placing the vacuum bag filled with the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor into a curing tank to carry out in-situ curing on the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor, wherein the in-situ curing temperature is 250 ℃, and the in-situ curing time is 4 hours, so as to obtain a carbon fiber composite material; and finally, taking the carbon fiber composite material out of the vacuum bag, and then putting the carbon fiber composite material into a medium-pressure cracking furnace to perform high-temperature medium-pressure cracking for 3 hours at the temperature of 1000 ℃ and under the pressure of 4MPa in a nitrogen atmosphere.
The density of the high-performance C/SiBCN composite material prepared by the embodiment is 1.91g/cm 3 The room-temperature bending strength was 505MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 373MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 587MPa.
Example 3
(1) The carbon fiber preform with a carbon cloth laminated sewing structure is adopted, and the density of the preform is 0.65-0.80 g/cm 3 Preparing C and SiC alternating interface layers C/SiC/C/SiC/C/SiC by adopting a CVI process (CVI), wherein the deposition time of each C interface layer is 10 hours, and the deposition time of each SiC interface layer is 15 hours, so as to obtain the modified carbon fiber preform.
(2) The preparation method comprises the following steps of taking a liquid SiBCN precursor (liquid polyborosilazane) as an impregnation liquid, adopting a PIP (Poly-p-phenylene-bis-phenyl) process of vacuum impregnation/in-situ curing/medium-pressure cracking to perform SiBCN matrix densification on a modified carbon fiber preform, and performing vacuum impregnation, in-situ curing and medium-pressure cracking, wherein the PIP process is a PIP process of one-step vacuum impregnation/in-situ curing/medium-pressure cracking; the cycle number of the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking is 6, so that the high-performance C/SiBCN composite material is obtained; the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking at each time specifically comprises the following steps: placing the modified carbon fiber preform in a vacuum bag, taking the liquid SiBCN precursor as impregnation liquid for vacuum impregnation, after vacuum impregnation for 2h, placing the vacuum bag filled with the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor into a curing tank to carry out in-situ curing on the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor, wherein the in-situ curing temperature is 250 ℃, and the in-situ curing time is 4 h, so as to obtain a carbon fiber composite material; and finally, taking the carbon fiber composite material out of the vacuum bag, and then putting the carbon fiber composite material into a medium-pressure cracking furnace to perform high-temperature medium-pressure cracking for 3 hours at the temperature of 1000 ℃ and under the pressure of 4MPa in a nitrogen atmosphere.
The density of the high-performance C/SiBCN composite material prepared by the embodiment is 1.95g/cm 3 The room-temperature bending strength was 720MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 541MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 766MPa.
The micro-topography (SEM image) of the high-performance C/SiBCN composite material prepared in this example is shown in fig. 1, and it can be known from the result of fig. 1 that the C/SiBCN composite material prepared in this example has fewer internal pores and denser micro-topography; the stress-strain curve at room temperature of the high-performance C/SiBCN composite material prepared in this example is shown in fig. 2, and as can be seen from the stress-strain curve in fig. 2, the room-temperature bending strength of the C/SiBCN composite material is greater than 700MPa, and the dispersion is small, which is related to the uniform densification of the internal structure of the composite material, and the small number of pores and cracks, and the high-performance C/SiBCN composite material is in a plastic fracture mode.
In particular, the 5 stress-strain curves in FIG. 2 show the results of testing five samples of the high performance C/SiBCN composite prepared in this example.
Example 4
Example 4 is essentially the same as example 3, except that: in this embodiment, the step (1) is not included, that is, C and SiC alternating interface layers C/SiC/C/SiC are not prepared on the surface of the carbon fiber preform with the carbon cloth laminated stitched structure, but liquid polyborosilazane is directly used as a liquid SiBCN precursor, and the liquid SiBCN precursor is used as an impregnation solution, and the same PIP process of vacuum impregnation/in-situ curing/medium pressure cracking as in embodiment 3 is performed.
The density of the C/SiBCN ceramic matrix composite material prepared by the embodiment is 1.90g/cm 3 The room-temperature bending strength was 401MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 289MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 476MPa.
Comparative example 1
(1) A three-dimensional orthogonal structure T700 carbon fiber fabric is used as a reinforcement to prepare a 100mm multiplied by 100mm flat plate sample, and the volume fraction of the fabric fiber is 45%.
(2) And (2) adopting liquid polyborosilazane as a SiBCN precursor, and introducing the SiBCN precursor into the carbon fiber fabric prepared in the step (1) by a vacuum impregnation method. And (2) impregnating the impregnation liquid into the fabric at 60 ℃ and under the pressure of 0.2MPa for 2 hours, taking out the blank after complete impregnation, putting the blank into a curing tank (60 ℃), performing pressure curing at the temperature of 200 ℃ and under the pressure of 3MPa for 8 hours, and slowly cooling along with a furnace until the precursor is completely cured.
(3) And (3) pyrolysis, namely putting the blank solidified in the step (2) into a high-temperature medium-pressure cracking furnace, and carrying out pyrolysis for 3 hours at 1000 ℃ and under 4MPa in a nitrogen atmosphere to finish the high-temperature conversion of the SiBCN organic polymer precursor to SiBCN.
(4) And (5) repeating the steps (2) and (3) for 6 times to finally obtain the compact SiBCN ceramic matrix composite.
The density of the SiBCN ceramic matrix composite material prepared by the comparative example is 1.82g/cm 3 The room-temperature bending strength was 364MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 231MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 396MPa.
Comparative example 2
Comparative example 2 is substantially the same as example 3 except that:
in the step (2), a liquid polyborosilazane precursor (liquid SiBCN precursor) is used as an impregnation liquid, and the conventional general PIP process is carried out; the circulation frequency of the PIP process is 6 times, and the C/SiBCN ceramic matrix composite material is obtained; each PIP process specifically comprises the following steps: placing the modified carbon fiber preform in a liquid SiBCN precursor for vacuum impregnation, taking the modified carbon fiber preform which is subjected to vacuum impregnation with the liquid SiBCN precursor out of an impregnation liquid after vacuum impregnation for 2 hours, and then placing the modified carbon fiber preform into a curing tank for curing, wherein the curing temperature is 250 ℃, and the curing time is 4 hours, so as to obtain a carbon fiber composite material; and finally, putting the carbon fiber composite material into a cracking furnace to carry out high-temperature normal-pressure cracking for 3 hours at 1000 ℃ in a nitrogen atmosphere.
The density of the C/SiBCN ceramic matrix composite material prepared by the comparative example is 1.83g/cm 3 The room-temperature bending strength was 409MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 283MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 436MPa.
Comparative example 3
Comparative example 3 is substantially the same as comparative example 2 except that:
the comparative example does not include the step (1), namely C/SiC/C/SiC/C/SiC of the C and SiC alternating interface layer is not prepared on the surface of the carbon fiber preform with the carbon cloth laminated sewing structure, but liquid polyborosilazane is directly adopted as a liquid SiBCN precursor, the liquid SiBCN precursor is adopted as an impregnation liquid, and the PIP process which is the same as that of the comparative example 2 is carried out.
The density of the C/SiBCN ceramic matrix composite material prepared by the comparative example is 1.86g/cm 3 The room-temperature bending strength was 275MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 195MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 284MPa.
Comparative example 4
Comparative example 4 is substantially the same as example 3 except that:
in the step (2), a liquid SiBCN precursor (liquid polyborosilazane) is used as an impregnation liquid, a PIP (poly-p-phenylene-bis-p-phenylene) process of vacuum impregnation/in-situ curing/normal pressure cracking is adopted to carry out SiBCN matrix densification on the modified carbon fiber preform, and vacuum impregnation, in-situ curing and normal pressure cracking are carried out, wherein the process is a PIP process of primary vacuum impregnation/in-situ curing/normal pressure cracking; the cycle times of the PIP process of vacuum impregnation/in-situ curing/normal-pressure cracking are 6 times, so that the C/SiBCN ceramic matrix composite is obtained; the PIP process of vacuum impregnation/in-situ curing/normal pressure cracking at each time specifically comprises the following steps: placing the modified carbon fiber preform in a vacuum bag, taking the liquid SiBCN precursor as impregnation liquid for vacuum impregnation, after vacuum impregnation for 2h, placing the vacuum bag filled with the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor into a curing tank to carry out in-situ curing on the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor, wherein the in-situ curing temperature is 250 ℃, and the in-situ curing time is 4 hours, so as to obtain a carbon fiber composite material; and finally, taking the carbon fiber composite material out of the vacuum bag, and then placing the carbon fiber composite material in a cracking furnace to perform high-temperature normal-pressure cracking for 3 hours at the temperature of 1000 ℃ in a nitrogen atmosphere.
The density of the C/SiBCN ceramic matrix composite material prepared by the comparative example is 1.87g/cm 3 The room-temperature bending strength was 418MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 288MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 454MPa.
Comparative example 5
Comparative example 5 is substantially the same as example 3 except that:
in the step (2), a liquid SiBCN precursor (liquid polyborosilazane) is used as an impregnation liquid, a PIP (poly-p-phenylene-bis-p-phenylene) process of vacuum impregnation/curing/medium-pressure cracking is adopted to carry out SiBCN matrix densification on the modified carbon fiber preform, and vacuum impregnation, curing and medium-pressure cracking are carried out, wherein the process is a PIP process of one-time vacuum impregnation/curing/medium-pressure cracking; the circulation frequency of the PIP process of vacuum impregnation/curing/medium-pressure cracking is 6 times, so that the C/SiBCN ceramic matrix composite is obtained; the PIP process of vacuum impregnation/curing/medium-pressure cracking at each time is specifically as follows: placing the modified carbon fiber preform in a liquid SiBCN precursor for vacuum impregnation, taking the modified carbon fiber preform which is subjected to vacuum impregnation with the SiBCN precursor out of an impregnation liquid after vacuum impregnation for 2h, and then placing the modified carbon fiber preform into a curing tank for curing, wherein the curing temperature is 250 ℃, and the curing time is 4 hours, so as to obtain the carbon fiber composite material; and finally, placing the carbon fiber composite material in a high-temperature medium-pressure cracking furnace, and carrying out high-temperature medium-pressure cracking for 3 hours at 1000 ℃ in a nitrogen atmosphere with the pressure of 4MPa.
The density of the C/SiBCN ceramic matrix composite material prepared by the comparative example is 1.88g/cm 3 The room-temperature bending strength was 428MPa, the bending strength after 3 hours at 1000 ℃ in an air atmosphere (the bending strength at 1000 ℃ in an air atmosphere) was 290MPa, and the bending strength after 3 hours at 1400 ℃ in an inert atmosphere (the bending strength at 1400 ℃ in an inert atmosphere) was 456MPa.
Compared with the example 3, the comparative example 2, the comparative example 3, the comparative example 4 and the comparative example 5, the mechanical property of the C/SiBCN composite material can be obviously improved when the modified carbon fiber preform with the interface layer is subjected to SiBCN matrix densification by the PIP process of vacuum impregnation/in-situ curing/medium-pressure cracking, and the C/SiBCN composite material prepared by the method has better high-temperature oxidation resistance and high-temperature mechanical property.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A preparation method of a high-performance C/SiBCN composite material is characterized by comprising the following steps:
(1) Preparing a C/SiC/C/SiC/C/SiC alternating interface layer formed by alternately depositing a C interface layer and a SiC interface layer on the surface of the carbon fiber preform to obtain a modified carbon fiber preform;
(2) Performing SiBCN matrix densification on the modified carbon fiber preform by taking a liquid SiBCN precursor as an impregnation liquid through a PIP (poly-p-phenylene-diisocyanate) process of vacuum impregnation/in-situ curing/medium-pressure cracking to obtain a high-performance C/SiBCN composite material; the liquid SiBCN precursor is liquid polyborosilazane;
the PIP process of vacuum impregnation/in-situ curing/medium pressure cracking comprises the following substeps:
(a) Placing the modified carbon fiber preform in a vacuum bag, and taking the liquid SiBCN precursor as impregnation liquid for vacuum impregnation; the vacuum impregnation time is 1.5-3 h;
(b) Putting a vacuum bag filled with the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor into a curing tank to carry out in-situ curing on the modified carbon fiber preform vacuum-impregnated with the liquid SiBCN precursor, so as to obtain a carbon fiber composite material; the temperature of the in-situ curing is 180-280 ℃, and the time of the in-situ curing is 3-6 h;
(c) Taking the carbon fiber composite material out of the vacuum bag and then placing the carbon fiber composite material in a medium-pressure cracking furnace for high-temperature medium-pressure cracking; carrying out high-temperature medium-pressure cracking in a nitrogen atmosphere or an argon atmosphere, wherein the temperature of the high-temperature medium-pressure cracking is 800-1100 ℃, the pressure of the high-temperature medium-pressure cracking is 3-6 MPa, and the time of the high-temperature medium-pressure cracking is 2-7 h;
the density of the high-performance C/SiBCN composite material is not less than 1.9g/cm 3 The room temperature bending strength is not lower than 700MPa, the bending strength under the air atmosphere of 1000 ℃ is not lower than 500MPa, and the bending strength under the inert atmosphere of 1400 ℃ is not lower than 650MPa.
2. The method of claim 1, wherein:
repeating the step (2) for 4-6 times.
3. The production method according to claim 1, characterized in that:
the density of the modified carbon fiber preform is 0.2-0.80 g/cm 3 。
4. The production method according to claim 1, characterized in that:
the viscosity of the liquid SiBCN precursor is less than 20mPa · s.
5. A high-performance C/SiBCN composite material produced by the production method according to any one of claims 1 to 4.
6. Use of the high-performance C/SiBCN composite material obtained by the production method according to any one of claims 1 to 4 as a thermostructural composite material.
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| CN112500180B (en) * | 2020-12-13 | 2022-10-11 | 中国航空制造技术研究院 | Nitride fiber reinforced ceramic-based wave-transparent composite material and precision forming method thereof |
| CN112745146B (en) * | 2021-01-11 | 2022-07-12 | 上海大学 | Local defect whisker or sheet reinforcing and repairing method of carbon/carbon composite material coating and repairing coating |
| CN113149680A (en) * | 2021-05-13 | 2021-07-23 | 尚辰(浙江绍兴)复合材料科技有限公司 | Carbon fiber reinforced silicon-boron-carbon-nitrogen-based ceramic composite material and preparation method thereof |
| CN113354432B (en) * | 2021-06-25 | 2023-01-24 | 上海大学 | Composite material with carbon matrix combined with silicon-boron-carbon-nitrogen matrix and preparation method thereof |
| CN113943175B (en) * | 2021-10-25 | 2022-12-27 | 西北工业大学 | Si-B-C gradient anti-oxidation coating of carbon/carbon composite material and preparation method thereof |
| WO2022174624A1 (en) * | 2021-11-02 | 2022-08-25 | 航天材料及工艺研究所 | High-temperature-resistant and oxidation-resistant light-weight heat-insulation foam material and preparation method therefor |
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