CN112341204B - Continuous fiber interweaved and laminated zirconium diboride-based composite material and preparation method thereof - Google Patents
Continuous fiber interweaved and laminated zirconium diboride-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of ultra-high temperature ceramic-based composite materials, and particularly relates to a continuous fiber interweaving and laminating zirconium diboride-based composite material and a preparation method thereof. The invention has the advantages that: the prepared composite material has low porosity, high strength, excellent fracture resistance, thermal shock resistance and oxidation resistance, and the method is simple and controllable to operate and easy to realize large-scale production.
Description
Technical Field
The invention belongs to the field of ultra-high temperature ceramic matrix composite materials, and particularly relates to a preparation method of a continuous fiber interweaved and laminated zirconium diboride matrix composite material.
Background
The continuous fiber toughened zirconium diboride-based composite material not only has the characteristics of high-temperature stability, high strength, high modulus and the like of zirconium diboride, but also has good thermal shock resistance (the strength of 300MPa can be kept at 1400 ℃), high fracture toughness and high fracture work (the fracture toughness is 10MP DEG, and the fracture work is 1000J/m2) Light weight (density 4 g/cm)3) And the like, and is expected to be used in extreme environments (temperature)>1600 c aerobic environment) is in service in hypersonic aircraft.
The continuous fiber changes the trend of cracks and absorbs fracture energy through toughening mechanisms such as fiber extraction, fiber debonding and fiber bridging, changes the inherent brittle catastrophic failure mode of zirconium diboride, and improves the reliability of the zirconium diboride in practical application. But the continuous fiber toughened zirconium diboride-based composite material has obvious anisotropy; the room temperature bending strength of the fiber in the 0 degree direction is 300MPa, while the bending strength of the fiber in the 90 degree direction (only 70MPa) is very low compared with the bending strength (500 MPa) of the ultra-high temperature ceramic substrate, which can be avoided by interweaving the fibers in different directions. However, due to the low self-diffusion coefficient and high melting point of zirconium diboride, it is difficult to uniformly distribute the matrix among the individual fibers during sintering. Often, the matrix is distributed on the periphery of the single fiber bundle, and the matrix content is less or even no more towards the interior of the fiber bundle. The prepared unidirectional fiber toughened zirconium diboride-based composite material has high porosity (> 10%) and contains a large number of defects, and zirconium diboride is sensitive to the defects, so that the strength of the obtained composite material is low. The preparation of the unidirectional fiber toughening zirconium diboride-based composite material with low porosity and excellent mechanical property is difficult, and the preparation of the zirconium diboride-based composite material with low porosity, high strength and high toughness interweaving continuous fibers in different directions is more difficult. In addition, for zirconium diboride-based ceramics with zirconium disilicide as a sintering aid, at 1400 ℃, the strength is severely reduced (from room temperature of 500MPa to 80MPa) due to the softening of zirconium disilicide, resulting in insufficient bearing capacity under extreme environments. Therefore, it is urgently needed to solve the above problems to realize the practical application of the continuous fiber toughened zirconium diboride-based composite material, so as to promote the further development of the advanced technology using the hypersonic aircraft as the background.
Disclosure of Invention
In order to overcome the problem that the preparation of the continuous fiber toughened zirconium diboride-based composite material in different interweaving directions is difficult and improve the bearing capacity and reliability of the composite material in a high-temperature environment, the technical scheme is as follows:
a preparation method of a continuous fiber interweaving and laminating zirconium diboride-based composite material utilizes the characteristic that polyether sulfone-zirconium diboride-based ceramic slurry is changed from liquid state to solid state when meeting water, continuous fibers dipped with the polyether sulfone-zirconium diboride-based ceramic slurry are put into the water for solidification and then are cold pressed into a continuous fiber single-layer plate, then the continuous fiber single-layer plate is sequentially layered at angles of 0 degree, 45 degrees, 90 degrees and 45 degrees to prepare a unit laminated plate, a plurality of unit laminated plates are stacked to prepare a pre-sintered green body, and finally the continuous fiber interweaving and laminating zirconium diboride-based composite material is prepared by hot-pressing and sintering, and the specific steps comprise:
1) preparing zirconium diboride-based ceramic slurry: adding 6.99-48.76 parts by mass of zirconium diboride, 0.13-5.8 parts by mass of zirconium carbide, 0.06-2.76 parts by mass of silicon carbide, 0.01-5 parts by mass of zirconium dihydride and 0.47-8.41 parts by mass of zirconium disilicide nano-scale powder into 20-200 parts by mass of 1-methyl-2-pyrrolidone, and ultrasonically oscillating for 60-180min under continuous mechanical stirring to uniformly mix;
2) preparing polyether sulfone-zirconium diboride-based ceramic slurry: dissolving 5-40 parts by mass of polyether sulfone in 20-200 parts by mass of 1-methyl-2-pyrrolidone at the temperature of 50-80 ℃, cooling, adding the zirconium diboride-based ceramic slurry obtained in the step 1), and continuously mechanically stirring for 60-180 min;
3) preparing a continuous fiber single-layer board: dipping the continuous fibers subjected to degumming treatment with the mass parts of 1.72-13.78 into the polyether sulfone-zirconium diboride-based ceramic slurry obtained in the step 2), and vacuumizing for 30-120min under the assistance of ultrasound to enable the polyether sulfone-zirconium diboride-based ceramic slurry to be filled among single fibers; then putting into deionized water for curing for 1-5min, and then cleaning for 3-15min with the assistance of ultrasonic waves by using absolute ethyl alcohol to remove 1-methyl-2-pyrrolidone; finally, placing the single-layer board into a metal mould, and pressing the single-layer board of the continuous fiber by applying pressure of 15-300 MPa;
4) preparing a pre-sintered blank: laminating the continuous fiber single-layer plates obtained in the step 3) at angles of 0 degree, 45 degrees, 90 degrees and 45 degrees to prepare a unit laminated plate, circularly stacking a plurality of unit laminated plates, dipping zirconium diboride-based ceramic slurry, and applying pressure of 30-200MPa to prepare a pre-sintered blank;
5) hot-pressing and sintering: placing the pre-sintered blank obtained in the step 4) in a vacuum hot-pressing sintering furnace, firstly vacuumizing to below 7Pa, then filling argon to above 270Pa, then vacuumizing again, and repeating for 3 times so as to reduce the oxygen content in the vacuum hot-pressing sintering furnace; after the vacuum reaches below 0.1Pa, applying and maintaining the pressure of 1-5MPa, raising the temperature to 600 ℃ at the heating rate of 5-8 ℃/min, and maintaining for 20-40min to remove the polyether sulfone; then raising the temperature to 900 ℃ at the heating rate of 8-15 ℃/min, applying the pressure of 30-50MPa, and keeping the pressure for 10-40 min; finally, the temperature is raised to 1300-1700 ℃ and the sintering is carried out for 30-120min, thus obtaining the continuous fiber interweaving and laminating zirconium diboride-based composite material.
The invention has the beneficial effects that:
1. according to the invention, the fiber after degumming treatment is immersed in the polyether sulfone-zirconium diboride-based ceramic slurry, under the ultrasonic-assisted and vacuum environment, the polyether sulfone-zirconium diboride-based ceramic slurry well enters the interior of a fiber bundle, so that the porosity of the composite material is effectively reduced, and the polyether sulfone has good rheological property at the temperature of 400 ℃ below zero, so that the flowing of a matrix is promoted to fill in the residual gaps, the densification of the composite material is facilitated, and the mechanical property of the composite material is further facilitated to be improved;
2. the method utilizes the characteristic that the polyether sulfone-zirconium diboride-based ceramic slurry is changed from liquid state to solid state when meeting water, puts the continuous fibers dipped with the polyether sulfone-zirconium diboride-based ceramic slurry into water for solidification, then carries out cold pressing to prepare continuous fiber single-layer plates, and then carries out hot pressing sintering on pre-sintered blanks prepared by continuously stacking the continuous fiber single-layer plates to prepare the continuous fiber interwoven and laminated zirconium diboride-based composite material, and has the advantages of simple and controllable operation and easy realization of large-scale production;
3. according to the invention, zirconium carbide and silicon carbide are used as reinforcing phases, so that the strength of the composite material is improved; zirconium hydride is used for removing residual carbon left after polyether sulfone cracking, and the zirconium hydride reacts with the residual carbon to generate zirconium carbide nanocrystalline in situ, so that the strength of the composite material is further improved; in addition, the silicon carbide is easy to form a layer of glassy protective film on the surface of the composite material in a high-temperature aerobic environment, so that further diffusion of oxygen is hindered, and the oxidation resistance of the composite material is improved;
4. the continuous fibers are alternately distributed in the composite material in the angle sequence of 0 degree, 45 degrees, 90 degrees and 45 degrees, so that the anisotropy of the composite material is reduced, the fracture toughness and the fracture work of the composite material are improved, the thermal shock resistance of the composite material is improved, the brittle disaster damage mode is avoided, and the service reliability of the composite material in an extreme environment is improved.
Drawings
Fig. 1 is a schematic flow chart of a preparation process of a continuous fiber interweaved and laminated zirconium diboride-based composite material of an embodiment.
Detailed Description
The invention is further illustrated with reference to the following specific examples, without limiting the scope of the invention thereto.
The preparation method of the continuous fiber interwoven and laminated zirconium diboride-based composite material, which is described in the embodiment, is characterized in that polyether sulfone-zirconium diboride-based ceramic slurry is converted from a liquid state to a solid state when meeting water, continuous fibers impregnated with the polyether sulfone-zirconium diboride-based ceramic slurry are put into water for curing, then are subjected to cold pressing to prepare a continuous fiber single-layer plate, then the continuous fiber single-layer plate is sequentially layered at angles of 0 degree, 45 degrees, 90 degrees and 45 degrees to prepare a unit laminated plate, a plurality of unit laminated plates are stacked to prepare a pre-sintered body, and finally the continuous fiber interwoven and laminated zirconium diboride-based composite material is prepared through hot pressing and sintering, and the specific steps comprise:
1) preparing zirconium diboride-based ceramic slurry: adding 26.5 parts by mass of zirconium diboride, 2.25 parts by mass of zirconium carbide, 1.07 parts by mass of silicon carbide, 1.83 parts by mass of zirconium dihydride and 6.54 parts by mass of zirconium disilicide nano-scale powder into 200 parts by mass of 1-methyl-2-pyrrolidone, and ultrasonically oscillating for 120min under continuous mechanical stirring to uniformly mix;
2) preparing polyether sulfone-zirconium diboride-based ceramic slurry: dissolving 15 parts by mass of polyether sulfone in 100 parts by mass of 1-methyl-2-pyrrolidone at the temperature of 60 ℃, cooling, adding the zirconium diboride-based ceramic slurry obtained in the step 1), and continuously mechanically stirring for 100 min;
3) preparing a continuous fiber single-layer board: soaking 5.17 parts by mass of continuous carbon fibers subjected to degumming treatment into the polyether sulfone-zirconium diboride-based ceramic slurry obtained in the step 2), and vacuumizing for 60min under the assistance of ultrasound to enable the polyether sulfone-zirconium diboride-based ceramic slurry to be filled among single fibers; then putting into deionized water for curing for 3min, and then cleaning for 10min with the assistance of ultrasonic waves by using absolute ethyl alcohol to remove the 1-methyl-2-pyrrolidone; finally, placing the single-layer continuous fiber board into a metal mold, and applying pressure of 20MPa to press the single-layer continuous fiber board;
4) preparing a pre-sintered blank: laminating the continuous fiber single-layer plates obtained in the step 3) at angles of 0 degree, 45 degrees, 90 degrees and 45 degrees to prepare a unit laminated plate, circularly stacking a plurality of unit laminated plates, then soaking zirconium diboride-based ceramic slurry, and applying pressure of 100MPa to prepare a pre-sintered green body;
5) hot-pressing and sintering: placing the pre-sintered blank obtained in the step 4) in a vacuum hot-pressing sintering furnace, firstly vacuumizing to below 7Pa, then filling argon to above 270Pa, then vacuumizing again, and repeating for 3 times so as to reduce the oxygen content in the vacuum hot-pressing sintering furnace; after the vacuum reaches below 0.1Pa, applying and maintaining the pressure of 1MPa, raising the temperature to 600 ℃ at the heating rate of 5 ℃/min, and maintaining for 30min to remove the polyether sulfone; then raising the temperature to 900 ℃ at the heating rate of 10 ℃/min, applying the pressure of 40MPa, and keeping the pressure for 20 min; and finally, heating to 1600 ℃ and sintering for 30min to obtain the continuous fiber interweaved and laminated zirconium diboride-based composite material.
In conclusion, the composite material obtained by the preparation method of the continuous fiber interweaved and laminated zirconium diboride-based composite material has low porosity, high strength, excellent fracture resistance, thermal shock resistance and oxidation resistance, and the method is simple and controllable to operate and easy to realize large-scale production.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (2)
1. A preparation method of a continuous fiber interweaving and laminating zirconium diboride-based composite material is characterized in that continuous fibers soaked with polyether sulfone-zirconium diboride-based ceramic slurry are put into water to be cured by utilizing the characteristic that the polyether sulfone-zirconium diboride-based ceramic slurry is changed from liquid state to solid state when meeting water, then the continuous fibers are cold pressed to form continuous fiber single-layer plates, then the continuous fiber single-layer plates are sequentially laminated at the angles of 0 degree, 45 degrees, 90 degrees and 45 degrees to form a unit laminated plate, a plurality of unit laminated plates are stacked to form a pre-sintered blank body, and finally the continuous fiber interweaving and laminating zirconium diboride-based composite material is prepared by hot-pressing and sintering, and the specific steps comprise:
1) preparing zirconium diboride-based ceramic slurry: adding 6.99-48.76 parts by mass of zirconium diboride, 0.13-5.8 parts by mass of zirconium carbide, 0.06-2.76 parts by mass of silicon carbide, 0.01-5 parts by mass of zirconium dihydride and 0.47-8.41 parts by mass of zirconium disilicide nano-scale powder into 20-200 parts by mass of 1-methyl-2-pyrrolidone, and ultrasonically oscillating for 60-180min under continuous mechanical stirring to uniformly mix;
2) preparing polyether sulfone-zirconium diboride-based ceramic slurry: dissolving 5-40 parts by mass of polyether sulfone in 20-200 parts by mass of 1-methyl-2-pyrrolidone at the temperature of 50-80 ℃, cooling, adding the zirconium diboride-based ceramic slurry obtained in the step 1), and continuously mechanically stirring for 60-180 min;
3) preparing a continuous fiber single-layer board: dipping the continuous fibers subjected to degumming treatment with the mass parts of 1.72-13.78 into the polyether sulfone-zirconium diboride-based ceramic slurry obtained in the step 2), and vacuumizing for 30-120min under the assistance of ultrasound to enable the polyether sulfone-zirconium diboride-based ceramic slurry to be filled among single fibers; then putting into deionized water for curing for 1-5min, and then cleaning for 3-15min with the assistance of ultrasonic waves by using absolute ethyl alcohol to remove 1-methyl-2-pyrrolidone; finally, placing the single-layer board into a metal mould, and pressing the single-layer board of the continuous fiber by applying pressure of 15-300 MPa;
4) preparing a pre-sintered blank: laminating the continuous fiber single-layer plates obtained in the step 3) at angles of 0 degree, 45 degrees, 90 degrees and 45 degrees to prepare a unit laminated plate, circularly stacking a plurality of unit laminated plates, dipping zirconium diboride-based ceramic slurry, and applying pressure of 30-200MPa to prepare a pre-sintered blank;
5) hot-pressing and sintering: placing the pre-sintered blank obtained in the step 4) in a vacuum hot-pressing sintering furnace, firstly vacuumizing to below 7Pa, then filling argon to above 270Pa, then vacuumizing again, and repeating for 3 times so as to reduce the oxygen content in the vacuum hot-pressing sintering furnace; after the vacuum reaches below 0.1Pa, applying and maintaining the pressure of 1-5MPa, raising the temperature to 600 ℃ at the heating rate of 5-8 ℃/min, and maintaining for 20-40min to remove the polyether sulfone; then raising the temperature to 900 ℃ at the heating rate of 8-15 ℃/min, applying the pressure of 30-50MPa, and keeping the pressure for 10-40 min; finally, the temperature is raised to 1300-1700 ℃ and the sintering is carried out for 30-120min, thus obtaining the continuous fiber interweaving and laminating zirconium diboride-based composite material.
2. A continuous fiber interleaved laminated zirconium diboride based composite characterized in that said continuous fiber interleaved laminated zirconium diboride based composite is made by the process of claim 1.
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