CN106904952B - High-temperature-resistant high-strength alumina fiber reinforced composite material and preparation method thereof - Google Patents
High-temperature-resistant high-strength alumina fiber reinforced composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-temperature-resistant high-strength alumina fiber reinforced composite material and a preparation method thereof, wherein a two-dimensional cloth laying layer, a 2.5D woven or orthogonal three-dimensional woven continuous alumina fiber preform is used as a reinforcement, a matrix is prepared by using a double-nano composite impregnation liquid in which silica and alumina are uniformly mixed, and the matrix is subjected to vacuum pressure impregnation, micro-positive pressure medium-low temperature pre-curing, micro-positive pressure curing and atmosphere temperature programmed segmented heat treatment to finally obtain the alumina fiber reinforced composite material, wherein the mass ratio of the silica to the alumina in the composite material is 19: 1-12: 8, the volume content of the alumina fiber is 30-60%, the prepared composite material has high-temperature-resistant performance and high-temperature mechanical property, the density of the material is high, the room-temperature tensile strength of the material reaches 310 +/-30 MPa, the 1100 ℃ tensile strength reaches 135 +/-20 MPa, and the 1200 ℃ tensile strength reaches 90 +/-10 MPa, compared with the similar quartz fiber reinforced silica oxide/oxide composite material, the performance of the composite material is improved by 4-5 times.
Description
Technical Field
The invention relates to a high-temperature-resistant high-strength alumina fiber reinforced composite material and a preparation method thereof, belonging to the field of ceramic matrix composite material preparation.
Background
With the rapid development of aerospace industry and the upgrading and upgrading of weaponry in China, higher requirements of light weight, high strength and toughness, high reliability and temperature resistance level improvement are put forward for a material system, and advanced composite materials represented by continuous fiber reinforced ceramic matrix composite materials can achieve 30-50% weight reduction effect compared with traditional materials, have equivalent strength, good reliability and excellent high temperature resistance, and therefore are paid more and more extensive attention. In the present stage, the advanced composite material has become a mainstream material scheme for the design of the advanced aircraft, is more and more fully applied to bullets, arrows, stars and ships, and plays more and more remarkable roles in the fields of civil aircrafts, automobile industries, nuclear industries and the like. The oxide fiber reinforced oxide ceramic matrix composite is one of advanced composite materials, the fiber and the matrix of the composite are both mainly oxides, compared with the non-oxide fiber reinforced ceramic matrix composite, the composite has no problem of high-temperature oxidation, can work for a long time in a high-temperature aerobic environment, and cannot form catastrophic damage due to oxidation. Therefore, under the condition of long-time high-temperature-resistant aerobic environment, the oxide fiber reinforced oxide composite material is an important development direction. The alumina fiber reinforced composite material is expected to be applied to turbine engines, combustion chambers, antenna covers and the like because the use temperature of the fibers in the oxidizing atmosphere can reach more than 1400 ℃. (F.W.Zok.development sin oxide fiber compositions.J.Am.Ceram.Soc., 89,3309-3324, (2006), K.A.Keller, G.Jefferson, and R.J.Kerans.oxide-oxides compositions, in Handbook of ceramics compositions, editedby N.A.Bansal (Kluwer Academic,2005), pp.377-421).
At present, besides the silica-based composite material reinforced by quartz fiber, the alumina fiber reinforced composite material is a more studied oxide fiber reinforced oxide composite material. The quartz fiber reinforced silica-based composite material is the oxide fiber reinforced oxide composite material which is most developed and applied at present, and is generally prepared by a sol-gel method, but the material is not suitable for long-time use at a high temperature of over 1200 ℃ because the crystallization phenomenon of silica occurs at about 1200 ℃. The alumina fiber composite material has attracted much attention after the above application bottlenecks are highlighted, and the alumina fiber composite material mainly uses alumina fibers (i.e. fibers whose main component is alumina) as reinforcing fibers, but at present, no detailed report is found on the composition of the continuous alumina fiber reinforced oxide composite material and the preparation method thereof.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the high-temperature-resistant high-strength alumina fiber reinforced composite material which has excellent high-temperature-resistant performance and high-temperature mechanical property, high material density and good comprehensive performance.
The invention also aims to provide a preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material.
The above purpose of the invention is mainly realized by the following technical scheme:
the high-temperature-resistant high-strength alumina fiber reinforced composite material takes alumina fibers as a reinforcement and takes a complex-phase ceramic matrix formed by silica and alumina as a matrix, wherein the mass ratio of the silica to the alumina is 19: 1-12: 8, and the volume content of the alumina fibers is 30-60%.
In the high-temperature-resistant high-strength alumina fiber reinforced composite material, the alumina fiber reinforcement is an integral fabric formed by sewing or weaving continuous alumina fibers by a two-dimensional cloth laying method and a 2.5D or orthogonal three-dimensional method.
A preparation method of a high-temperature-resistant high-strength alumina fiber reinforced composite material comprises the following steps:
step one, carrying out purification heat treatment on the alumina fiber reinforcement;
mixing the nano silica sol and the nano alumina powder, and dispersing by ball milling or ultrasonic to form a composite impregnation liquid, wherein the viscosity of the composite impregnation liquid is 30-150 mPa & s;
step three, placing the purified and heat-treated alumina fiber reinforcement in the composite impregnation liquid for vacuum and pressure impregnation;
step four, pre-curing the alumina fiber reinforcement impregnated with the composite impregnation liquid at the temperature of below 250 ℃;
step five, carrying out segmented heat treatment on the pre-cured alumina fiber reinforcement at 800-1200 ℃ to densify the alumina fiber reinforcement, so as to obtain an alumina fiber reinforced composite material blank;
and (VI), repeating the steps (three) to (five) on the aluminum oxide fiber reinforced composite material blank, and finishing the preparation process when the weight gain of the aluminum oxide fiber reinforced composite material blank is less than or equal to 2 wt% to obtain the final aluminum oxide fiber reinforced composite material.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the alumina fiber reinforcement in the step (I) is an integral fabric formed by sewing or weaving continuous alumina fibers by a two-dimensional cloth laying method and a 2.5D or orthogonal three-dimensional method; the volume content of the alumina fiber reinforcement is 30-60%.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the purification heat treatment temperature in the step (I) is 380-750 ℃, and the heat treatment time is 0.5-8 h.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the specific method for forming the composite impregnation liquid in the step (two) is as follows:
mixing nano alumina powder and deionized water in a mass ratio of 30: 100-1.5: 100, adding a dispersing agent to obtain a nano alumina powder suspension, and mixing the nano silica sol and the nano alumina powder suspension according to a mass ratio of 5: 1-0.2: 1, and then dispersing by adopting a ball milling or ultrasonic method to form the composite impregnation liquid.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, SiO in the nano silica sol2The solid phase mass percentage content of (1) is 15-45%, SiO2The size of (A) is 10-100 nm; the size of the nano alumina powder is 50-300 nm.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the dispersing agent is CELUNAD-305, BYK-154 or BYK-191; the mass of the dispersing agent is 0.05-6.0% of the mass of the nano alumina powder.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the ball milling speed is 600-1200 r/min, and the ball milling time is 10-200 min.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, in the step (three), vacuum impregnation and pressure impregnation are alternately performed for 1-3 times, the vacuum degree of the vacuum impregnation is 10-200 Pa, and the impregnation time is 30-180 min; the pressure adopted by pressure impregnation is 0.15-4.5 MPa, and the impregnation time is 30-180 min.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the pre-curing in the step (IV) is carried out in two stages under the micro-positive pressure of 0.15-0.75 MPa, the atmosphere is air or nitrogen, the pre-curing in the first stage is carried out at the temperature of 110-150 ℃, the heat preservation time is 1-4 hours, the pre-curing in the second stage is carried out at the temperature of 200-250 ℃, and the heat preservation time is 1-10 hours.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the step (V) of the segmented heat treatment is performed by adopting temperature programming and segmentation, and the specific heat treatment conditions are as follows: the temperature is between room temperature and 800 ℃, the heat treatment atmosphere is air, the flow rate of the air is controlled to be 0.05-5L/min, the heating rate is 0.05-6 ℃/min, and the heat preservation time is 2-8 h; 800-target highest temperature, wherein the heat treatment atmosphere is nitrogen, the flow rate of the nitrogen is 0.05-5L/min, and the heating rate is 0.05-6 ℃/min; the heat preservation time is 2-8 h at the target maximum heat treatment temperature.
In the preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material, the target maximum temperature is 1000-1300 ℃.
Compared with the prior art, the invention has the following beneficial effects:
(1) the material system design of the invention takes alumina fiber as a reinforcement, alumina and silicon oxide complex phase ceramic as a substrate, and obtains uniform double nano composite impregnation liquid in a chemical modification and physical ball milling mode, the density of the material and the retention rate of powder are improved by a low-temperature pre-curing process under vacuum pressure, and a high-temperature oxidation resistant composite material with excellent room temperature and high-temperature mechanical properties is finally obtained by a circulating impregnation heat treatment method, and the material density is high.
(2) The material system of the invention selects a complex phase ceramic form of silicon dioxide and aluminum oxide on the design of the substrate, and can adjust the modulus and the linear expansion coefficient of the composite material by adjusting the proportion of the silicon dioxide and the aluminum oxide, thereby improving the thermal matching between the fiber and the substrate.
(3) The impregnation phase adopted by the invention is a double-nano composite impregnation liquid, namely, the composite impregnant is prepared from silica sol, nano alumina powder, a dispersing agent and deionized water, and the nano alumina powder is uniformly introduced into the impregnation liquid by selecting the dispersing agent, so that the solid phase volume content in the impregnation liquid is improved, and the impregnation efficiency is improved; the nano alumina powder has higher sintering activity, the retention rate of alumina components in the composite material is improved, and the density of the material is greatly improved; compared with the method of separately dipping silica sol and nano alumina powder or dipping silica sol and micron alumina powder, the dipping efficiency is improved by 40-70%, and the density of the material is improved by 15-38%.
(4) According to the invention, a micro-positive pressure medium-low temperature pre-curing method is adopted in the curing stage, so that the volume expansion and the formation of pores in the curing process can be effectively inhibited, the density of the material is greatly improved, and compared with a normal pressure curing mode, the density of the material is improved by 10-20%.
(5) The method adopts air and nitrogen atmosphere for segmented heat treatment densification in the heat treatment densification stage, can effectively inhibit the creep phenomenon of the fiber in a high-temperature area, and improves the tensile strength at 1400 ℃ by 20-30% compared with the whole segment adopting air heat treatment.
(6) The alumina fiber reinforced composite material prepared by the invention has excellent high temperature resistance and high temperature mechanical property, the room temperature tensile strength reaches 310 +/-30 MPa, the modulus is adjustable within 90-150 MPa, and the thermal expansion coefficient is (1-5) multiplied by 10-6The tensile strength at 1100 ℃ is 135 +/-20 MPa, the tensile strength at 1200 ℃ is 90 +/-10 MPa, the tensile strength at 1400 ℃ is 70 +/-10 MPa, and the tensile strength at 1500 ℃ is 60 +/-10 MPa; compared with a quartz fiber reinforced silicon dioxide-based composite material, the room-temperature tensile strength of the alumina fiber reinforced oxide composite material is improved by 200-350%, and the tensile strength at 1200℃ is improvedThe degree is improved by 300-400%, and the tensile strength at 1400 ℃ and 1500 ℃ is qualitatively improved.
Drawings
FIG. 1 shows the microstructure of a room-temperature tensile fracture of a high-temperature-resistant and high-strength alumina fiber reinforced composite material in example 1 of the present invention;
FIG. 2 shows the microstructure of 1500 ℃ tensile fracture of the high temperature resistant and high strength alumina fiber reinforced composite material in example 2 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
the high-temperature-resistant high-strength alumina fiber reinforced composite material takes alumina fibers as a reinforcement and takes a complex phase ceramic matrix formed by silica and alumina as a matrix, wherein the mass ratio of the silica to the alumina is 19: 1-12: 8, the volume content of the alumina fibers is 30-60%, and the volume content of the complex phase ceramic matrix formed by the silica and the alumina is 70-40%. The alumina fiber reinforcement is an integral fabric formed by sewing or weaving continuous alumina fibers by a two-dimensional cloth laying method and a 2.5D or orthogonal three-dimensional method. The composite material can be expressed as Al2O3f/SiO2-Al2O3。
The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material comprises the following steps:
and (I) taking a continuous alumina fiber prefabricated body formed by sewing or weaving a two-dimensional cloth laying layer and a 2.5D or orthogonal three-dimensional method as a reinforcement, wherein the volume content of the fiber reinforcement is 30-60%.
And (II) putting the alumina fiber preform prepared in the step (I) into a muffle furnace for purification heat treatment, wherein the heat treatment temperature is 380-750 ℃, and the heat treatment time is 0.5-8 h.
And (III) mixing the nano alumina powder and deionized water according to a mass ratio of 30: 100-1.5: 100, adding 0.05-6.0% of dispersing agent, wherein the dispersing agent is CELUNA D-305 (Mikyo grease Co., Ltd.), BYK-154 (Pico chemistry) or BYK-191 (Pico chemistry), performing ultrasonic treatment for 10-120 min until a uniform dispersion liquid is formed, then mixing the nano silica sol and the nano alumina powder suspension according to the mass ratio of 5: 1-0.2: 1, performing ball milling or ultrasonic treatment for dispersion, wherein the rotating speed of a ball mill is 600-1200 r/min, the ball milling time is 10-200 min, and the double nano composite impregnation liquid with stable viscosity and uniform dispersion is formed, and can be used when the viscosity of the impregnation liquid reaches 30-150 mPa · s.
SiO in nano silica sol2The solid phase mass percentage content of (1) is 15-45%, SiO2The size of (A) is 10-100 nm; the size of the nano alumina powder is 50-300 nm.
Step four, placing the alumina fiber preform obtained in the step two into the double-nano composite impregnation liquid obtained in the step three, and impregnating by a vacuum state and pressure state circulating impregnation method, wherein the vacuum degree of vacuum impregnation is 10-200 Pa, and the impregnation time is 30-180 min; the pressure of pressure impregnation is 0.15-4.5 MPa, and the impregnation time is 30-180 min. And alternately carrying out vacuum impregnation and pressure impregnation for 1-3 times.
And (V) carrying out micro-positive pressure pre-curing treatment on the alumina preform obtained in the step (IV) by using an impregnation liquid, wherein the curing process is respectively carried out under the micro-positive pressure of 0.15-0.75 MPa, the atmosphere is air or nitrogen, the pre-curing in the first stage is carried out at 110-150 ℃, the pre-curing in the second stage is carried out at 200-250 ℃, the heat preservation time of the two temperature stages is 1-4 h and 1-10 h respectively, and the total pre-curing time is 2-14 h respectively. The micro positive pressure in the present invention is a positive pressure 1.1 to 2.0 times the atmospheric pressure.
Step (VI), performing segmented heat treatment at 800-1200 ℃ to densify to obtain the aluminum oxide fiber reinforced composite material blank, wherein the segmented heat treatment is performed by temperature programming and segmentation, the highest temperature of the heat treatment densification is 1000-1300 ℃, and the specific heat treatment conditions are as follows: the heat treatment atmosphere at room temperature to 800 ℃ is air, the flow rate of the air is controlled to be 0.05 to 5L/min, the heating rate is 0.05 to 6 ℃/min, and the heat preservation time is 2 to 8 hours; the heat treatment atmosphere at the maximum temperature of 800-target (1000-1300 ℃) is nitrogen, the flow rate of the nitrogen is 0.05-5L/min, and the heating rate is 0.05-6 ℃/min; the heat preservation time is 2-8 h at the target maximum heat treatment temperature (namely 1000-1300 ℃).
And (seventhly), repeating the step (four) to the step (six) for 3-10 times, and when the weight gain of the aluminum oxide fiber composite blank is less than or equal to 2 wt% (namely the ratio of the increased mass to the mass before weight gain is multiplied by 100%), finishing the densification process to obtain the dense aluminum oxide fiber reinforced composite.
The material system of the invention is designed by taking high-strength alumina fiber as a reinforcement, and forming a complex phase ceramic matrix by silica and alumina according to a certain proportion, wherein the mass ratio (m) of the silica to the aluminaSiO2:mAl2O3) The controllable range is 19: 1-12: 8. When the matrix is completely composed of silicon dioxide, although the modulus of the material can be effectively reduced, the thermal expansion coefficient of the material is different from that of the alumina fiber of the reinforcement by an order of magnitude, when the composite material is subjected to high temperature, the thermal mismatch is generated due to the difference of the thermal expansion coefficients of the two, so that a plurality of microcracks are easily generated inside the composite material at high temperature, and the high-temperature mechanical property of the material is greatly reduced. After a certain proportion of alumina is added into the matrix, the thermal expansion coefficient of the matrix can be improved, and the thermal mismatch between the fiber and the matrix is greatly reduced; and secondly, the nano alumina powder and the silica sol form a homogeneous structure, so that the sintering performance is better, and the density of the composite material can be effectively improved. In the dipping process, the double-nano composite dipping solution is adopted, and a process of low-temperature pre-curing in vacuum pressure is adopted, so that the density of the material and the retention rate of powder can be greatly improved, and the density of the material is improved by 15-38%. Finally, the high-strength alumina fiber reinforced composite material with excellent high-temperature resistance can be obtained, the room-temperature tensile strength of the material reaches 310 +/-45 MPa, the modulus is adjustable within 90-150 MPa, and the thermal expansion coefficient is (1-5) multiplied by 10-6The tensile strength at 1100 ℃ is 135 +/-20 MPa, the tensile strength at 1200 ℃ is 90 +/-10 MPa, the tensile strength at 1400 ℃ is 70 +/-10 MPa, and the tensile strength at 1500 ℃ is 60 +/-10 MPa; the alumina fiber reinforced oxide composite has improved room temperature tensile strength compared to quartz fiber reinforced silica-based compositesThe tensile strength is increased by 200-350%, the tensile strength at 1200 ℃ is increased by 300-400%, and the tensile strength at 1400 ℃ and 1500 ℃ is improved qualitatively.
Aiming at the application of the composite material in a long-time high-temperature aerobic environment, the invention adopts high-strength oxidation-resistant alumina fiber as a reinforcement and adopts oxide ceramic as a matrix, so that the material has good high-temperature resistance and high-temperature oxidation resistance. Because the alumina fiber has high modulus, when the composite material is used as a component, the modulus of the composite material needs to be adjusted, so that the matrix design adopts a complex phase ceramic form of silicon dioxide and alumina, wherein the silicon dioxide can adjust the modulus of the composite material, the alumina can adjust the thermal matching between the fiber and the matrix, and the silicon dioxide and the alumina form a complex phase ceramic matrix according to a certain proportion, wherein the mass ratio of the silicon dioxide to the alumina (m is the mass ratio of the silicon dioxide to the alumina)SiO2:mAl2O3) Controllable in the range of 19: 1-12: 8, and the material system is abbreviated as Al2O3f/SiO2-Al2O3。
The aluminum oxide prefabricated body adopts a two-dimensional cloth laying layer and a 2.5D or orthorhombic three-way weaving structure, and the 2.5D and orthorhombic three-way weaving prefabricated body is an integral fabric and does not need other treatment; the two-dimensional cloth is layered with the alumina fiber preform, the XY direction is the two-dimensional cloth woven by alumina fiber, and the Z direction is punctured or sewed by alumina fiber. The volume content of the preform fiber is 30-60%. The prefabricated body is subjected to purification treatment before subsequent steps, high-temperature heat treatment at 380-750 ℃ is generally adopted, and the heat treatment time is 0.5-8 h.
Example 1
(1) Taking a 2.5D continuous alumina fiber prefabricated body as a reinforcement, wherein the volume content of the fiber is 42%;
(2) placing the alumina fiber preform prepared in the step (1) into a muffle furnace for purification heat treatment, wherein the heat treatment temperature is 700 ℃, and the heat treatment time is 5 hours;
(3) mixing nano alumina powder and deionized water according to the mass ratio of 28:100, adding 3.5% of dispersing agent CELUNA D-305, and performing ultrasonic treatment for 100min to form uniform dispersion liquid; then, mixing the nano silica sol with the solid phase content of 40% and the nano alumina powder suspension according to the mass ratio of 1: 1.5, placing the mixture in a ball mill, wherein the rotating speed of the ball mill is 800r/min, the ball milling time is 100min, and the viscosity of the impregnation liquid is 120mPa & s after uniform mixing;
(4) placing the alumina fiber preform obtained in the step (2) into the double-nano composite impregnation liquid obtained in the step (3), vacuum impregnating for 120min, wherein the vacuum degree is 133Pa, and then carrying out pressure impregnation, wherein the impregnation pressure is 1.25MPa, and the impregnation time is 120 min;
(5) firstly, carrying out first-stage pre-curing on the alumina preform obtained in the step (4) at 130 ℃, wherein the curing pressure is 0.70MPa, the atmosphere is air, and the pre-curing time is 3.5 h; then, the second stage of pre-curing is carried out at 240 ℃, the curing pressure is 0.70MPa, the atmosphere is air, and the curing time is 6 h.
(6) And (3) carrying out temperature programming and sectional heat treatment on the alumina fiber preform obtained in the step (5) in the air and nitrogen atmosphere. The heat treatment atmosphere at room temperature to 800 ℃ is air, the flow rate of the air is controlled to be 2.5L/min, the heating rate is 5 ℃/min, the heat preservation time is 4h, the heat treatment atmosphere at 800 to 1200 ℃ is nitrogen, the flow rate of the nitrogen is 2.5L/min, the heating rate is 5 ℃/min, and the heat preservation time is 3h at 1200 ℃;
(7) repeating the steps (3) - (6) for 6 times, wherein the weight gain is less than or equal to 2 wt%, and the densification process is finished to obtain the final alumina fiber reinforced ceramic matrix composite material, namely Al2O3f/SiO2-Al2O3。
The properties of the alumina fiber reinforced ceramic matrix composite of this example are as follows:
the density of the composite material is 2.61g/cm3The room-temperature tensile strength was 282MPa, the modulus was 130MPa, the 1200 ℃ tensile strength was 94MPa, the 1400 ℃ tensile strength was 70MPa, and the 1500 ℃ tensile strength was 61MPa, respectively.
As shown in fig. 1, the microstructure of the high temperature resistant and high strength alumina fiber reinforced composite at room temperature tensile fracture in example 1 of the present invention, and as shown in fig. 2, the microstructure of the high temperature resistant and high strength alumina fiber reinforced composite at 1500 ℃ tensile fracture in example 2 of the present invention, it can be seen from the figure that the composite is compact, and after undergoing a room temperature tensile property test, the fracture exhibits an obvious fiber pull-out phenomenon and exhibits a ductile fracture mode; after the material is subjected to a 1500 ℃ high-temperature tensile property test, the fracture still presents a certain fiber pull-out effect, which is proved that the material has good high-temperature mechanical properties.
Example 2
(1) Taking a continuous alumina fiber prefabricated body with two-dimensional cloth laying as a reinforcement, wherein the volume content of the fiber is 38%;
(2) placing the alumina fiber preform prepared in the step (1) into a muffle furnace for purification heat treatment, wherein the heat treatment temperature is 400 ℃, and the heat treatment time is 3 hours;
(3) and mixing the nano alumina powder and deionized water in a ratio of 15: mixing 100 mass percent, adding 2.0 percent of dispersing agent CELUNA D-305, and carrying out ultrasonic treatment for 60min to form uniform dispersion liquid; then, mixing the nano silica sol with the solid phase content of 40% and the nano alumina powder suspension according to the mass ratio of 1: 1, placing the mixture in a ball mill, wherein the rotating speed of the ball mill is 600r/min, the ball milling time is 60min, and the viscosity of the impregnation liquid after uniform mixing is 50mPa & s;
(4) placing the alumina fiber preform obtained in the step (2) into the double-nano composite impregnation liquid obtained in the step (3), vacuum impregnating for 1h with the vacuum degree of 100Pa, and then carrying out pressure impregnation with the impregnation pressure of 0.2MPa for 1 h;
(5) and (3) firstly pre-curing the alumina preform obtained in the step (4) at 110 ℃, wherein the pre-curing pressure in the first stage is 0.5MPa, the atmosphere is air, and the pre-curing time is 2h, and then, pre-curing in the second stage is carried out at 200 ℃, the curing pressure is 0.2MPa, the atmosphere is air, and the curing time is 4 h.
(6) And (3) carrying out temperature programming and sectional heat treatment on the alumina fiber preform obtained in the step (5) in the air and nitrogen atmosphere. The heat treatment atmosphere at room temperature to 800 ℃ is air, the flow rate of the air is controlled to be 1.5L/min, the heating rate is 2 ℃/min, and the heat preservation time is 2 h; the heat treatment atmosphere at 800-1000 ℃ is nitrogen, the flow rate of the nitrogen is 2L/min, and the heating rate is 2 ℃/min; keeping the temperature at 1000 ℃ for 3 h;
(7) repeating the steps (3) - (6) for 6 times, wherein the weight gain is less than or equal to 2 wt%, and the densification process is finished to obtain the final alumina fiber reinforced ceramic matrix composite material, namely Al2O3f/SiO2-Al2O3。
The properties of the alumina fiber reinforced ceramic matrix composite of this example are as follows:
the density of the composite material is 2.26g/cm3Tensile strength at room temperature of 267MPa, modulus of 115MPa, and coefficient of thermal expansion of 3.7X 10-6and/K, the tensile strength at 1200 ℃ is 84MPa, the tensile strength at 1400 ℃ is 62MPa, and the tensile strength at 1500 ℃ is 54MPa respectively.
The above description is only for the best mode of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Those skilled in the art will appreciate that the invention may be practiced without these specific details.
Claims (9)
1. A preparation method of a high-temperature-resistant high-strength alumina fiber reinforced composite material is characterized by comprising the following steps: the method comprises the following steps:
step one, carrying out purification heat treatment on the alumina fiber reinforcement;
mixing the nano silica sol and the nano alumina powder, and dispersing by ball milling or ultrasonic to form a composite impregnation liquid, wherein the viscosity of the composite impregnation liquid is 30-150 mPa & s;
step three, placing the purified and heat-treated alumina fiber reinforcement in the composite impregnation liquid for vacuum and pressure impregnation;
step four, pre-curing the alumina fiber reinforcement impregnated with the composite impregnation liquid at the temperature of below 250 ℃;
step five, carrying out segmented heat treatment on the pre-cured alumina fiber reinforcement at 800-1200 ℃ to densify the alumina fiber reinforcement, so as to obtain an alumina fiber reinforced composite material blank;
step (VI), repeating the step (three) to the step (five) on the aluminum oxide fiber reinforced composite material blank, and finishing the preparation process when the weight gain of the aluminum oxide fiber reinforced composite material blank is less than or equal to 2 wt% to obtain the final aluminum oxide fiber reinforced composite material;
the specific method for forming the composite impregnation liquid in the step (II) is as follows:
mixing nano alumina powder and deionized water in a mass ratio of 30: 100-1.5: 100, adding a dispersing agent to obtain a nano alumina powder suspension, and mixing the nano silica sol and the nano alumina powder suspension according to a mass ratio of 5: 1-0.2: 1, and then dispersing by adopting a ball milling or ultrasonic method to form a composite impregnation liquid;
and (3) carrying out pre-curing in the step (IV) under the micro-positive pressure of 0.15-0.75 MPa in two stages, wherein the atmosphere is air or nitrogen, the pre-curing in the first stage is carried out at the temperature of 110-150 ℃, the heat preservation time is 1-4 h, the pre-curing in the second stage is carried out at the temperature of 200-250 ℃, and the heat preservation time is 1-10 h.
2. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 1, characterized by comprising the following steps: the alumina fiber reinforcement in the step (one) is an integral fabric formed by sewing or weaving continuous alumina fibers by a two-dimensional cloth laying method and a 2.5D or orthogonal three-dimensional method; the volume content of the alumina fiber reinforcement is 30-60%.
3. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 1, characterized by comprising the following steps: in the step (I), the purification heat treatment temperature is 380-750 ℃, and the heat treatment time is 0.5-8 h.
4. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 1, characterized by comprising the following steps: SiO in the nano silica sol2The solid phase mass percentage content of (1) is 15-45%, SiO2The size of (A) is 10-100 nm; the size of the nano alumina powder is 50-300 nm.
5. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 1, characterized by comprising the following steps: the dispersing agent is CELUNA D-305, BYK-154 or BYK-191; the mass of the dispersing agent is 0.05-6.0% of the mass of the nano alumina powder.
6. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 1, characterized by comprising the following steps: the rotating speed of the ball milling is 600-1200 r/min, and the ball milling time is 10-200 min.
7. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 1, characterized by comprising the following steps: in the step (III), vacuum impregnation and pressure impregnation are alternately carried out for 1-3 times, the vacuum degree of the vacuum impregnation is 10-200 Pa, and the impregnation time is 30-180 min; the pressure adopted by pressure impregnation is 0.15-4.5 MPa, and the impregnation time is 30-180 min.
8. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 1, characterized by comprising the following steps: the step (V) of the segmented heat treatment adopts temperature programming and is performed in a segmented way, and the specific heat treatment conditions are as follows: the temperature is between room temperature and 800 ℃, the heat treatment atmosphere is air, the flow rate of the air is controlled to be 0.05-5L/min, the heating rate is 0.05-6 ℃/min, and the heat preservation time is 2-8 h; 800-target highest temperature, wherein the heat treatment atmosphere is nitrogen, the flow rate of the nitrogen is 0.05-5L/min, and the heating rate is 0.05-6 ℃/min; the heat preservation time is 2-8 h at the target maximum heat treatment temperature.
9. The preparation method of the high-temperature-resistant high-strength alumina fiber reinforced composite material according to claim 8, characterized in that: the target maximum temperature is 1000-1300 ℃.
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