CN115196984A - Three-dimensional woven alumina fiber reinforced oxide ceramic matrix composite containing interface phase and preparation method thereof - Google Patents
Three-dimensional woven alumina fiber reinforced oxide ceramic matrix composite containing interface phase and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of alumina fiber reinforced oxide ceramic composite materials, and relates to a three-dimensional woven interface modified continuous alumina fiber reinforced oxide ceramic matrix composite material and a preparation method thereof. The preparation method comprises the following steps: firstly, weaving a three-dimensional structure alumina fiber prefabricated body compounded with oxide powder; taking poly zirconium yttrium oxygen alkane as precursor solution, adopting precursor dipping pyrolysis method to obtain Yttria Stabilized Zirconia (YSZ) interface; and taking an oxide organic polymer as a precursor solution, soaking the pyrogenic composite oxide matrix again by adopting the precursor, and sintering at high temperature to obtain the alumina fiber reinforced oxide ceramic matrix composite material containing the YSZ weak interface. The YSZ weak interface significantly improves the composite strength, fracture toughness and damage tolerance. The precursor impregnation pyrolysis method adopted by the invention can greatly avoid fiber corrosion and high-temperature damage, and can realize net size forming to obtain a high-density matrix.
Description
Technical Field
The invention relates to a three-dimensional woven interface phase-containing alumina fiber reinforced oxide ceramic matrix composite and a preparation method thereof, belonging to the technical field of composite preparation.
Background
The continuous fiber reinforced ceramic matrix composite material has higher toughness and damage tolerance, and mainly comprises the following functions of a toughening mechanism:
(1) Fiber debonding and extraction mechanism
Under the action of an external stress, the matrix transmits partial stress to the high-modulus fibers, so that the load borne by the matrix material is reduced, when the stress borne by the fibers exceeds the strength of the fibers, the fibers break and slide in the matrix, interfacial debonding occurs, and finally the fibers are pulled out.
(2) Crack deflection mechanism
When the continuous fiber reinforced ceramic matrix composite material is stressed, a substrate cracks, and when the continuous fiber reinforced ceramic matrix composite material meets fibers in the expansion process, due to the interface effect of the fibers and the substrate, the cracks expand along the interface, namely deflect along the surface of the fibers to form a zigzag path, so that the energy is consumed, and the toughening effect is achieved.
(3) Bridging effect
The bridging effect means that the crack propagates in the matrix, and the fiber at the tail end of the crack is not broken so as to form a fiber bridging area, namely the bridging effect, and the existence of the area causes the crack to consume more energy in the process of propagating so as to realize toughening.
The residual compressive stress of the interface of the alumina ceramic matrix composite is larger, so that the interface bonding force of the fiber and the matrix is stronger, the toughening behaviors of fiber debonding and pulling out are limited, and the improvement of the toughness and the improvement of the fracture mode of the composite are not facilitated. In order to optimize the interfacial property of the composite material and obtain the composite material with high toughness and high strength, the YSZ coating is deposited on the fiber to be used as an interfacial layer to provide a weak interface to promote crack deflection, and the debonding and pulling-out behaviors of the fiber are stimulated to realize toughening. The YSZ interface layer deposited on the surface of the fiber fabric makes the interlayer bonding weaker, and cracks are easy to generate and delaminate. Due to the introduction of the YSZ weak interface layer, cracks are generated in the matrix and then are expanded to the fiber layer, the fiber layer can deflect and further expand along the interface layer with weaker combination between the fibers and the matrix, the fibers slide under the action of stress, a large amount of energy is absorbed, the debonding and the pulling-out of the fibers are realized, and the fracture toughness of the composite material is improved.
Patent CN106699209 relates to a preparation method of a continuous alumina fiber reinforced alumina ceramic matrix composite. The main steps of the technology are that the fiber fabric is repeatedly dipped and cracked in the oxide organic polymer to obtain an organic coating, the slurry is coated on the surface of the fiber fabric, the fiber fabric is placed in a mould to be laminated in vacuum, frozen and solidified, and freeze-dried to obtain a blank framework, the blank framework is placed in an inorganic alumina precursor to be dipped in vacuum and freeze-dried, the operations are repeated, and finally the composite material is obtained by high-temperature sintering. In the patent, the slurry is coated on the surface of the fiber fabric and then is put into a mold for pressurization, so that the phenomenon of macroscopic difference of fiber density and sparseness of the composite material caused by uneven distribution of fibers and a matrix can be generated, and the mechanical property of the composite material can be influenced to a certain extent by the unevenness; the alumina fiber of this patent is woven into three-dimensional overall structure, and the base member is filled in the pyrolysis, can not produce the dense and sparse macroscopical difference phenomenon of fibre, not only is showing the intensity and the toughness that have improved combined material, still can realize the net size shaping, and the material performance is excellent.
Patent CN108892522 relates to a preparation method of an oxide fiber reinforced oxide porous ceramic matrix composite. The preparation method comprises the main steps of preparing slurry, coating the slurry on the surface of a fiber fabric, drying to obtain a prepreg, carrying out vacuum hot pressing to obtain a preformed body, and sintering at high temperature to obtain the composite material. Patent CN110467439 relates to a preparation method of alumina fiber reinforced porous alumina ceramic matrix composite. The preparation method mainly comprises the steps of preparing slurry by using a precursor and alumina powder, coating the slurry on the surface of a fiber fabric, drying to obtain a prepreg, carrying out hot pressing in a vacuum press to obtain a preformed body, and finally sintering to obtain the porous alumina ceramic matrix composite. In the above patent, after the slurry is coated on the surface of the fiber, no further substrate densification process is needed, and the fiber is directly sintered at high temperature, so that no dense substrate exists in the fiber fabric, and the performance of the composite material is poor. The preparation method utilizes the oxide organic ceramic polymer precursor solution to repeatedly dip, cure and pyrolyze to obtain a more compact matrix, and the composite material has better performance.
Disclosure of Invention
The invention aims to provide a method for preparing a three-dimensional woven interface-phase-containing alumina fiber reinforced oxide ceramic matrix composite with a high matrix density, mainly aiming at a three-dimensional woven interface-phase-containing alumina fiber reinforced oxide ceramic matrix composite which is used in a high-temperature water-oxygen environment for a long time and has good performance, particularly higher toughness and a preparation method thereof.
The technical scheme of the invention is as follows: the method comprises the following operation steps:
1) Preparation of three-dimensional prefabricated body of alumina fiber composite oxide powder
Dissolving oxide powder in ethanol, wherein the mass fraction of the oxide powder is 45-55%, and putting the mixture into a planetary ball mill for ball milling for 6-24 hours to obtain oxide powder slurry; putting the alumina fiber into the oxidized slurry, and performing vacuum impregnation; and (3) after the impregnation is finished, removing the solvent from the fiber in an oven, wherein the heat treatment temperature is 80-200 ℃, and the time is 2-3 hours, so that the alumina fiber compounded with the oxide powder is obtained. Weaving alumina fiber compounded with oxide powder into a three-dimensional prefabricated body of the compound oxide powder with a three-dimensional structure;
(2) Preparation of three-dimensional prefabricated body YSZ interface
Placing the three-dimensional prefabricated body in a poly-zirconium-yttrium-oxygen-alkane organic matter precursor for vacuum and pressure impregnation; after the impregnation is finished, placing the three-dimensional preform in a vacuum oven for solvent removal treatment, curing a poly-zirconium-yttrium-oxygen-alkane organic precursor on the surface of the fiber fabric, and then performing high-temperature pyrolysis in a muffle furnace, wherein the pyrolysis process is 600-900 ℃, repeating the precursor impregnation-curing-pyrolysis process for 1-5 times on the three-dimensional preform until a YSZ interface with the thickness of 500-1000nm is obtained on the surface of the alumina fiber fabric, and then performing the precursor impregnation-curing process again;
(3) Preparation of composite matrices
And (3) taking an oxide organic polymer as a precursor solution, and adopting a precursor impregnation pyrolysis technology to generate an oxide matrix in situ in the three-dimensional preform. Dipping the fiber preform into an oxide organic polymer precursor solution with the solid content of 40-60wt% for vacuum and pressure dipping; then, putting the dipped prefabricated member into a vacuum oven for curing at the curing temperature of 150-250 ℃ for 2-10h; putting the cured prefabricated member into a high-temperature pyrolysis furnace for pyrolysis, and introducing argon for protection during vacuum pyrolysis, wherein the pyrolysis temperature is 500-900 ℃, and the heat preservation time is 1-3h; repeating the processes of dipping, curing and cracking until the weight of the composite material after dipping and drying is not more than 1 percent, and preparing a composite material blank with a compact matrix;
(4) Sintering of composite green bodies
And (3) sintering the composite material blank with the compact matrix prepared in the step in a high-temperature furnace at the sintering temperature of 1100-1300 ℃ for 1-5h to finally obtain the three-dimensional woven alumina fiber reinforced oxide ceramic matrix composite.
The oxide powder mainly comprises one or two of alumina and mullite powder, the particle size of the oxide powder is 100-1000nm, and the mass fraction of the oxide powder in the three-dimensional preform of the alumina fiber composite oxide powder is 6-20%.
The alumina fiber fabric is a three-dimensional integral braided fabric, and the three-dimensional structure of the alumina fiber fabric is one of a unidirectional ply structure, a 2.5D shallow cross-direct structure and a three-dimensional four-way structure. 30-60% of the volume content of the alumina three-dimensional preform.
Vacuum impregnation is carried out firstly, and then pressure impregnation is carried out, so that the impregnation efficiency is improved, and the slurry is promoted to enter the three-dimensional prefabricated body.
The high temperature pyrolysis temperature of the poly (zirconyl yttrium oxide) is 600-900 ℃ in order to avoid fiber damage under high temperature conditions.
The oxide organic polymer precursor solution is one or a mixture of two of polyaluminoxane and polyaluminosiloxane.
The oxide organic ceramic-based polymer precursor is an organic matter, does not have acidity or alkalinity, and can avoid the damage of alumina fibers.
The unidirectional ply structure is formed by weaving alumina fibers in a weft direction and ES fibers in a warp direction.
The 2.5D shallow cross-direct structure and the three-dimensional four-way structure are woven by alumina fibers without ES fibers.
The invention has the advantages that:
1. the invention adopts the poly-zirconium-yttrium-oxygen alkane to prepare the fiber interface, and the organic matter has no acidity or alkalinity and does not react with the fiber, thereby avoiding the damage of the alumina fiber.
2. The invention adopts the oxide organic ceramic polymer precursor to prepare a compact matrix, and can avoid the damage of alumina fibers under the high-temperature condition.
3. The sintering temperature of the composite material is not more than 1300 ℃, which is favorable for reducing fiber damage and maintaining the strength of the fiber, thereby improving the strength of the composite material.
4. The YSZ is used as the coating of the alumina fiber, so that a weak interface is formed on the surface of the alumina fiber, the crack deflection and the debonding and pulling-out of the fiber are facilitated, and the fracture toughness of the ceramic matrix composite is improved.
5. The invention has flexible structural design to the composite material, can realize the structural control of the composite material by changing the fiber weaving mode, and achieves the aim of different use requirements.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present specification and which fall within the limits of the appended claims.
Example 1
Putting 500nm alumina powder and ethanol into a planetary ball mill according to the mass ratio of 1: 1, performing ball milling for 12 hours to obtain a uniform solution, performing vacuum impregnation on alumina fibers in the uniform solution for 30 minutes, drying in a 150 ℃ oven for 3 hours to obtain alumina fibers compounded with the alumina powder, and weaving into a three-dimensional preform with a 2.5D shallow cross-direct structure. Treating the three-dimensional preform in a high-temperature furnace at 500 ℃ for 4 hours, removing glue on the surface of the alumina fiber, vacuum-impregnating the fiber fabric in poly (zirconium yttrium-siloxane) with the solid content of 40% and the viscosity of 350mPa.s for 1 hour, taking out the fiber fabric, and curing in a vacuum oven at 150 ℃ for 2 hours; putting the cured prefabricated member into a high-temperature pyrolysis furnace for pyrolysis, introducing argon for protection in vacuum pyrolysis, wherein the pyrolysis temperature is 600 ℃, and the heat preservation time is 3 hours; repeating the operation for 4 times to obtain a three-dimensional prefabricated body of a YSZ interface with the thickness of 600 nm; vacuum-impregnating the three-dimensional preform in polyaluminoxane with the solid content of 60% and the viscosity of 550mPa.s for 1 hour, pressure-impregnating under the pressure of 1.5Mpa for 3 hours, taking out the fiber fabric, and curing in a vacuum oven at the temperature of 200 ℃ for 3 hours; putting the cured prefabricated member into a high-temperature pyrolysis furnace for pyrolysis, introducing argon for protection in vacuum pyrolysis, wherein the pyrolysis temperature is 600 ℃, and the heat preservation time is 3 hours; the above operations are repeated for 12 times to obtain a composite material blank with a compact matrix.
And sintering the composite material in a high-temperature furnace at 1200 ℃ for 4 hours to obtain the 2.5D shallow cross-linked structure reinforced alumina fiber reinforced alumina ceramic matrix composite material containing the YSZ interface.
Example 2
Putting 50wt% of 1000nm mullite powder and 50wt% of ethanol into a planetary ball mill, performing ball milling for 24 hours to obtain a uniform solution, putting alumina fibers into the uniform solution, performing vacuum impregnation for 40 minutes, drying in an oven at 150 ℃ for 2 hours to obtain alumina fibers compounded with YSZ powder, and weaving the fibers into a three-dimensional four-way structure three-dimensional woven fabric; treating the three-dimensional prefabricated body in a high-temperature furnace at 600 ℃ for 4 hours, removing glue on the surface of the alumina fiber, carrying out vacuum impregnation on the fiber fabric in the zirconium-yttrium-siloxane with the solid content of 50% and the viscosity of 400mPa.s for 2 hours, taking out the fiber fabric, and curing in a vacuum oven at 180 ℃ for 2 hours; putting the cured prefabricated member into a high-temperature pyrolysis furnace for pyrolysis, introducing argon for protection in vacuum pyrolysis, wherein the pyrolysis temperature is 700 ℃, and the heat preservation time is 3 hours; repeating the operation for 5 times to obtain a three-dimensional prefabricated body of a YSZ interface with the thickness of 800 nm; vacuum-dipping the three-dimensional prefabricated body in polyaluminosiloxane with the solid content of 50% and the viscosity of 500mPa.s for 1 hour, pressure-dipping for 3 hours under the pressure of 2Mpa, taking out the fiber fabric, and curing for 4 hours in a vacuum oven at 180 ℃; putting the cured prefabricated member into a high-temperature pyrolysis furnace for pyrolysis, introducing argon for protection in vacuum pyrolysis, wherein the pyrolysis temperature is 700 ℃, and the heat preservation time is 3 hours; the above operations are repeated for 14 times to obtain a composite material blank with a compact matrix.
And (3) sintering the composite material in a high-temperature furnace at 1150 ℃ for 6 hours to obtain the alumina fiber reinforced mullite ceramic matrix composite material with the YSZ coating and the reinforced three-dimensional four-way structure.
Claims (4)
1. The three-dimensional woven alumina fiber reinforced oxide ceramic matrix composite containing the interface phase and the preparation method thereof are characterized in that:
the method comprises the following operation steps:
(1) Preparation of three-dimensional prefabricated body of alumina fiber composite oxide powder
Dissolving oxide powder in ethanol, wherein the mass fraction of the oxide powder is 45-55%, and putting the mixture into a planetary ball mill for ball milling for 6-24 hours to obtain oxide powder slurry; putting the alumina fiber into the oxidized slurry, and performing vacuum impregnation; and after the impregnation is finished, removing the solvent from the fiber in an oven, and performing heat treatment at the temperature of 80-200 ℃ for 2-3 hours to obtain the alumina fiber compounded with the oxide powder. Weaving alumina fiber compounded with oxide powder into a three-dimensional prefabricated body of three-dimensional composite oxide powder;
(2) Preparation of three-dimensional prefabricated body YSZ interface
Placing the three-dimensional prefabricated body in a poly-zirconium-yttrium-oxygen-alkane organic matter precursor for vacuum and pressure impregnation; after the impregnation is finished, placing the three-dimensional preform in a vacuum oven for solvent removal treatment, curing the poly-zirconium-yttrium-oxygen-alkane organic precursor on the surface of the fiber fabric, and then performing high-temperature pyrolysis in a muffle furnace, wherein the pyrolysis process is 600-900 ℃, repeating the precursor impregnation-curing-pyrolysis process for 1-5 times on the three-dimensional preform until a YSZ interface with the thickness of 500-1000nm is obtained on the surface of the alumina fiber fabric, and then performing the precursor impregnation-curing process again;
(3) Preparation of composite matrices
Taking an oxide organic polymer as a precursor solution, and adopting a precursor impregnation pyrolysis technology to generate an oxide matrix in situ in the three-dimensional preform. Dipping the fiber preform into an oxide organic polymer precursor solution with the solid content of 40-60wt% for vacuum and pressure dipping; then, putting the dipped prefabricated member into a vacuum oven for curing at the curing temperature of 150-250 ℃ for 2-10h; putting the cured prefabricated member into a high-temperature pyrolysis furnace for pyrolysis, and introducing argon for protection in vacuum pyrolysis at the pyrolysis temperature of 500-900 ℃ for 1-3h; repeating the processes of dipping, curing and cracking until the weight of the composite material after dipping and drying is not more than 1 percent, and preparing a composite material blank with a compact matrix;
(4) Sintering of composite green bodies
And (3) sintering the composite material blank with the compact matrix prepared in the step in a high-temperature furnace at the sintering temperature of 1100-1300 ℃ for 1-5h to finally obtain the three-dimensional woven alumina fiber reinforced oxide ceramic matrix composite.
2. The three-dimensional woven interface-containing alumina fiber reinforced oxide ceramic matrix composite and the method of making the same according to claim 1, wherein: the oxide powder in the step (1) is mainly one or two of alumina and mullite powder, the particle size of the oxide powder is 100-1000nm, and the mass fraction of the oxide powder in the three-dimensional preform of the alumina fiber composite oxide powder is 6-20%.
3. The three-dimensional woven alumina fiber reinforced oxide ceramic matrix composite with interface and the method for preparing the same according to claim 1, wherein: the alumina fiber fabric in the step (1) is a three-dimensional integral braided fabric, and the three-dimensional structure of the alumina fiber fabric is one of a unidirectional ply structure, a 2.5D shallow cross-linking structure and a three-dimensional four-way structure. 30-60% of the volume content of the aluminum oxide three-dimensional preform.
4. The three-dimensional woven interface-containing alumina fiber reinforced oxide ceramic matrix composite and method of making same according to claim 1, wherein the oxide organic polymer precursor solution is one or a mixture of polyaluminoxane and polyaluminosiloxane.
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| CN115636681A (en) * | 2022-10-26 | 2023-01-24 | 航天特种材料及工艺技术研究所 | Nitride fiber reinforced silicon nitride composite material and preparation method and application thereof |
| CN116102342A (en) * | 2023-02-24 | 2023-05-12 | 中国科学院兰州化学物理研究所 | High damage tolerance alumina composite ceramic and preparation method thereof |
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