CN109553431B - Preparation method of hollow quartz fiber fabric tough ceramic matrix composite material - Google Patents
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Abstract
The invention discloses a preparation method of a hollow quartz fiber fabric tough ceramic matrix composite, relates to a preparation method of a ceramic matrix composite, and aims to solve the problems of high density and low mechanical property of the existing aircraft thermal structure bearing material. The preparation method comprises the following steps: firstly, soaking a hollow quartz fiber fabric into an organic solvent for degumming; secondly, soaking the quartz fiber fabric subjected to the photoresist removal in an inorganic surface modifier solution to obtain a quartz fiber fabric subjected to surface protection treatment; dipping the quartz fiber fabric into a high-concentration ceramic aqueous solution, and then dipping the quartz fiber fabric into a low-concentration ceramic aqueous solution; fourthly, carrying out high-temperature dehydration treatment on the quartz fiber fabric at the temperature of 300-500 ℃; fifthly, sequentially repeating the dipping treatment in the third step and the pre-sintering in the fourth step; and sixthly, sintering at high temperature. The invention leads the fabric structure to be stable and the mechanical property to be excellent through surface protection treatment and dipping treatment, and the apparent density of the composite material is only 1.0 to 1.5g/cm3。
Description
Technical Field
The invention relates to a preparation method of a ceramic matrix composite.
Background
As the mach number of an aircraft increases, the heat resistance and wave transmission requirements on the main thermal bearing structure of the aircraft are higher and higher. The traditional resin-based composite material is far from meeting the heat-resistant requirement due to low heat-resistant temperature. Although the heat-resisting temperature is greatly improved, the density of the common ceramic materials, such as fused quartz ceramic, alumina ceramic, silicon nitride and the like, is higher, and the requirement of weight reduction of an aircraft cannot be met. The invention provides a preparation technology of a hollow quartz fiber fabric tough ceramic matrix composite, which can ensure the overall mechanical reliability and high-temperature heat resistance of the composite and simultaneously show excellent high-temperature wave-transmitting performance.
Disclosure of Invention
The invention aims to solve the problems of high density and low mechanical property of the existing aircraft thermal structure bearing material, and provides a preparation method of a hollow quartz fiber fabric tough ceramic matrix composite material.
The preparation method of the hollow quartz fiber fabric tough ceramic matrix composite material is realized according to the following steps:
firstly, hollow fabric quartz fiber surface photoresist removing treatment: soaking the hollow quartz fiber fabric in an organic solvent for degumming treatment to obtain a degumming quartz fiber fabric;
secondly, fiber surface protection treatment: soaking the quartz fiber fabric subjected to photoresist removal in an inorganic surface modifier solution, and drying to obtain a quartz fiber fabric subjected to surface protection treatment; wherein the inorganic surface modifier consists of 5 to 20 mass percent of aluminum hydroxide, 10 to 30 mass percent of aluminum nitrate, 5 to 25 mass percent of silicon hydroxide and 60 to 80 mass percent of deionized water;
thirdly, dipping the hollow fabric: dipping the quartz fiber fabric subjected to surface protection treatment into a ceramic aqueous solution with the concentration of 40-60 wt%, then dipping the quartz fiber fabric into a ceramic aqueous solution with the concentration of 10-30 wt%, and vacuumizing the dipping process to obtain the quartz fiber fabric subjected to dipping treatment;
fourthly, pre-sintering: carrying out high-temperature dehydration treatment on the impregnated quartz fiber fabric at the temperature of 300-500 ℃ for 1-3 h to obtain a hollow fabric tough ceramic matrix composite blank;
fifthly, sequentially repeating the dipping treatment and the pre-sintering process of the step three for multiple times until the quality of the pre-sintered composite material blank is not changed, and obtaining the pre-sintered composite material blank;
sixthly, high-temperature sintering: and (3) sintering the composite material blank subjected to the pre-sintering treatment at the temperature of 600-1000 ℃ for 1-2 h to obtain the hollow quartz fiber fabric tough ceramic matrix composite.
According to the invention, through the surface protection treatment in the second step and the dipping treatment in the third step, the standing property of the hollow fabric in the composite material is good, and the structure does not collapse, so that excellent mechanical properties are maintained, and meanwhile, due to the existence of the hollow structure, the apparent density of the composite material is lower, and the purpose of reducing weight is achieved.
The apparent density of the hollow quartz fiber fabric tough ceramic matrix composite material obtained by the invention is 1.0-1.5 g/cm3A compressive strength of more than 100MPa, a dielectric constant of 2 to 3, and a dielectric loss of less than 5X 10-3。
Detailed Description
The first embodiment is as follows: the preparation method of the hollow quartz fiber fabric tough ceramic matrix composite material is implemented according to the following steps:
firstly, hollow fabric quartz fiber surface photoresist removing treatment: soaking the hollow quartz fiber fabric in an organic solvent for degumming treatment to obtain a degumming quartz fiber fabric;
secondly, fiber surface protection treatment: soaking the quartz fiber fabric subjected to photoresist removal in an inorganic surface modifier solution, and drying to obtain a quartz fiber fabric subjected to surface protection treatment; wherein the inorganic surface modifier consists of 5 to 20 mass percent of aluminum hydroxide, 10 to 30 mass percent of aluminum nitrate, 5 to 25 mass percent of silicon hydroxide and 60 to 80 mass percent of deionized water;
thirdly, dipping the hollow fabric: dipping the quartz fiber fabric subjected to surface protection treatment into a ceramic aqueous solution with the concentration of 40-60 wt%, then dipping the quartz fiber fabric into a ceramic aqueous solution with the concentration of 10-30 wt%, and vacuumizing the dipping process to obtain the quartz fiber fabric subjected to dipping treatment;
fourthly, pre-sintering: carrying out high-temperature dehydration treatment on the impregnated quartz fiber fabric at the temperature of 300-500 ℃ for 1-3 h to obtain a hollow fabric tough ceramic matrix composite blank;
fifthly, sequentially repeating the dipping treatment and the pre-sintering process of the step three for multiple times until the quality of the pre-sintered composite material blank is not changed, and obtaining the pre-sintered composite material blank;
sixthly, high-temperature sintering: and (3) sintering the composite material blank subjected to the pre-sintering treatment at the temperature of 600-1000 ℃ for 1-2 h to obtain the hollow quartz fiber fabric tough ceramic matrix composite.
In the first step of the embodiment, the resin modified layer on the surface of the quartz fiber is removed by a solvent soaking method, wherein the used solvent comprises acetone, methanol and the like, and the first step is to prevent the dielectric property of the composite material from being deteriorated due to the high-temperature carbonization of the surface layer of the fiber.
The second embodiment is as follows: the difference between this embodiment and the first embodiment is that the organic solvent in the first step is acetone or methanol.
The third concrete implementation mode: the first or second embodiment is different from the first or second embodiment in that the time for the immersion photoresist removing treatment in the first step is 12 to 96 hours.
The fourth concrete implementation mode: the difference between the first embodiment and the third embodiment is that the quartz fiber fabric stripped in the second step is soaked in the inorganic surface modifier solution for 1-6 hours.
The fifth concrete implementation mode: the difference between the present embodiment and one of the first to fourth embodiments is that the temperature for drying in the second step is 25-100 ℃.
The sixth specific implementation mode: the difference between the present embodiment and one of the first to fifth embodiments is that the vacuum degree is controlled to be less than 10Pa during the vacuum pumping process in the third step.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is that the ceramic aqueous solution in step three is an alumina aqueous solution or a silica aqueous solution.
The specific implementation mode is eight: the difference between the first embodiment and the seventh embodiment is that in the third step, the quartz fiber fabric after surface protection treatment is dipped into a ceramic aqueous solution with the concentration of 40 wt% -60 wt% for 1-3 h, and then dipped into a ceramic aqueous solution with the concentration of 10 wt% -30 wt% for 1-3 h.
The specific implementation method nine: the present embodiment is different from the first to eighth embodiments in that the temperature rise rate is controlled to be 1 to 10 ℃/min in the fourth high-temperature dehydration treatment.
The detailed implementation mode is ten: the difference between the present embodiment and one of the first to ninth embodiments is that the step five sequentially repeats the dipping treatment and the pre-sintering process of the step three 6 to 10 times.
The concrete implementation mode eleven: the difference between the present embodiment and one of the first to tenth embodiments is that the temperature rise rate is controlled to be 1-5 ℃/min in the six-step high-temperature sintering process.
Example (b): the preparation method of the hollow quartz fiber fabric tough ceramic matrix composite material is implemented according to the following steps:
firstly, hollow fabric quartz fiber surface photoresist removing treatment: soaking the hollow quartz fiber fabric in an organic solvent acetone for 48h for degumming treatment to obtain a degumming quartz fiber fabric;
secondly, fiber surface protection treatment: soaking the quartz fiber fabric subjected to photoresist removal in an inorganic surface modifier solution for 2 hours, and drying to obtain a quartz fiber fabric subjected to surface protection treatment; wherein the inorganic surface modifier consists of 10 percent of aluminum hydroxide, 15 percent of aluminum nitrate, 5 percent of silicon hydroxide and 70 percent of deionized water according to mass percentage;
thirdly, dipping the hollow fabric: dipping the quartz fiber fabric subjected to surface protection treatment in a high-concentration 50 wt% ceramic aqueous solution for 1h, then dipping the quartz fiber fabric in a low-concentration 30 wt% ceramic aqueous solution for 1h, vacuumizing the dipping process, and controlling the vacuum degree to be less than 10Pa to obtain the quartz fiber fabric subjected to dipping treatment;
fourthly, pre-sintering: carrying out high-temperature dehydration treatment on the quartz fiber fabric subjected to the dipping treatment at the temperature of 400 ℃ for 2h to obtain a hollow fabric tough ceramic matrix composite blank;
fifthly, sequentially repeating the dipping treatment and the pre-sintering process of the step three for multiple times until the quality of the pre-sintered composite material blank is not changed, and obtaining the pre-sintered composite material blank;
sixthly, high-temperature sintering: and (3) sintering the composite material blank subjected to the pre-sintering treatment at the temperature of 1000 ℃ for 2h to obtain the hollow quartz fiber fabric tough ceramic matrix composite.
The apparent density of the hollow quartz fiber fabric tough ceramic matrix composite material obtained in the embodiment is 0.2g/cm3A compressive strength of 45MPa, a dielectric constant of 2.2 and a dielectric loss of 2.0X 10-3The heat-resisting temperature is more than 1200 ℃.
Claims (9)
1. The preparation method of the hollow quartz fiber fabric tough ceramic matrix composite material is characterized by comprising the following steps:
firstly, hollow fabric quartz fiber surface photoresist removing treatment: soaking the hollow quartz fiber fabric in an organic solvent for degumming treatment to obtain a degumming quartz fiber fabric;
secondly, fiber surface protection treatment: soaking the quartz fiber fabric subjected to photoresist removal in an inorganic surface modifier solution, and drying to obtain a quartz fiber fabric subjected to surface protection treatment; wherein the inorganic surface modifier consists of 5 to 20 mass percent of aluminum hydroxide, 10 to 30 mass percent of aluminum nitrate, 5 to 25 mass percent of silicon hydroxide and 60 to 80 mass percent of deionized water;
thirdly, dipping the hollow fabric: dipping the quartz fiber fabric subjected to surface protection treatment into a ceramic aqueous solution with the concentration of 40-60 wt%, then dipping the quartz fiber fabric into a ceramic aqueous solution with the concentration of 10-30 wt%, and vacuumizing the dipping process to obtain the quartz fiber fabric subjected to dipping treatment;
fourthly, pre-sintering: carrying out high-temperature dehydration treatment on the impregnated quartz fiber fabric at the temperature of 300-500 ℃ for 1-3 h to obtain a hollow fabric tough ceramic matrix composite blank;
fifthly, sequentially repeating the dipping treatment and the pre-sintering process of the step three for multiple times until the quality of the pre-sintered composite material blank is not changed, and obtaining the pre-sintered composite material blank;
sixthly, high-temperature sintering: sintering the composite material blank subjected to the pre-sintering treatment at the temperature of 600-1000 ℃ for 1-2 h to obtain the hollow quartz fiber fabric tough ceramic matrix composite;
wherein the ceramic water solution in the third step is alumina water solution or silica water solution.
2. The method for preparing the hollow quartz fiber fabric tough ceramic-based composite material according to claim 1, wherein the organic solvent in the first step is acetone or methanol.
3. The preparation method of the hollow quartz fiber fabric tough ceramic-based composite material according to claim 1, wherein the soaking and degumming treatment in the first step is carried out for 12-96 hours.
4. The preparation method of the hollow quartz fiber fabric tough ceramic-based composite material according to claim 1, wherein the quartz fiber fabric without glue in the second step is soaked in the inorganic surface modifier solution for 1-6 hours.
5. The preparation method of the hollow quartz fiber fabric tough ceramic matrix composite material according to claim 1, wherein the drying temperature in the second step is 25-100 ℃.
6. The method for preparing the hollow quartz fiber fabric tough ceramic-based composite material according to claim 1, wherein the vacuum degree is controlled to be less than 10Pa in the vacuum pumping process in the third step.
7. The preparation method of the hollow quartz fiber fabric tough ceramic-based composite material according to claim 1, characterized in that in the third step, the quartz fiber fabric after surface protection treatment is firstly soaked in a ceramic aqueous solution with the concentration of 40 wt% -60 wt% for 1-3 h, and then soaked in a ceramic aqueous solution with the concentration of 10 wt% -30 wt% for 1-3 h.
8. The preparation method of the hollow quartz fiber fabric tough ceramic-based composite material according to claim 1, wherein the temperature rise speed is controlled to be 1-10 ℃/min in the four-step high-temperature dehydration treatment.
9. The preparation method of the hollow quartz fiber fabric tough ceramic-based composite material according to claim 1, wherein the dipping treatment and the pre-sintering process in the third step are sequentially repeated for 6-10 times in the fifth step.
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| CN110590339B (en) * | 2019-09-30 | 2022-04-01 | 哈尔滨理工大学 | Preparation method of alumina ceramic component |
| CN114057475B (en) * | 2020-11-23 | 2022-11-11 | 航天特种材料及工艺技术研究所 | Silicon dioxide ceramic matrix composite material and preparation method thereof |
| CN113896554B (en) * | 2021-10-09 | 2023-03-17 | 航天特种材料及工艺技术研究所 | High-density fiber reinforced quartz ceramic composite material and preparation method thereof |
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