CN117865660A - Preparation method of zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material - Google Patents

Preparation method of zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material Download PDF

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CN117865660A
CN117865660A CN202311735496.2A CN202311735496A CN117865660A CN 117865660 A CN117865660 A CN 117865660A CN 202311735496 A CN202311735496 A CN 202311735496A CN 117865660 A CN117865660 A CN 117865660A
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carbon fiber
continuous carbon
composite material
zirconia
drying
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张乐
陈士卫
王婷
陈东顺
邱凡
康健
张馨元
陈浩
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Jiangsu Xiyi High Tech Materials Industry Technology Research Institute Co ltd
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Abstract

The invention discloses a preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material, which comprises the following steps: soaking the continuous carbon fiber in acetone, washing with distilled water, and drying in an oven; immersing the dried continuous carbon fiber into pure methanol completely, stirring ultrasonically, and then placing the separated continuous carbon fiber into an oven until the continuous carbon fiber is dried completely; mixing fused quartz powder, zirconia powder and a dispersing agent in ionized water, and performing ball milling to obtain an impregnating material; impregnating the pretreated continuous carbon fibers into an impregnating material to obtain an impregnated composite material; stacking the materials in a graphite mold, and hot-pressing and sintering under nitrogen atmosphere to obtain the composite material. The method has the advantages of simple process, short molding time and low cost, and can effectively increase the interfacial bonding strength of the carbon fiber and the quartz ceramic matrix and the bending strength perpendicular to the fiber direction in the prepared composite material, and the obtained composite material has good high-temperature stability and self-healing performance.

Description

Preparation method of zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material
Technical Field
The invention relates to preparation of a quartz ceramic matrix composite material, in particular to a preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material.
Background
With the acceleration of the development pace of aerospace, high-performance continuous fiber reinforced ceramic matrix composites are receiving more and more attention. In the field of space lightweight structural materials, carbon fiber reinforced glass matrix composites exhibit a wide range of characteristics including high strength, high stiffness, excellent toughness, low density, unique wear resistance, environmental stability, and the like. Fused silica is characterized by its significantly low density (2.2 g/cm 3 ) The glass substrate material has the characteristics of low thermal expansion coefficient, low heat conductivity coefficient, high softening temperature, excellent chemical inertness and the like, and is one of glass substrate materials for heat insulation boards and space light-weight structures. Pure fused silica is rarely used due to its inherent brittleness and very low mechanical properties. The bending strength of the high-performance continuous carbon fiber reinforced ceramic matrix composite is tens of times that of pure fused quartz, the fracture toughness is improved by 3 orders of magnitude, but the mechanical properties are anisotropic. Namely, the bending strength in the direction parallel to the fiber can reach 600MPa, but the strength perpendicular to the fiber is lower than 20MPa.
The patent with publication number CN103482994A discloses a preparation method of a carbon fiber reinforced quartz ceramic matrix composite, which is characterized in that carbon fibers are immersed in quartz powder and silica sol, and the carbon fiber reinforced quartz matrix composite is prepared through mechanical processing, but the bending strength of the carbon fiber reinforced quartz matrix composite perpendicular to the fiber direction is still smaller, the anisotropy of mechanical properties exists, and the density batch of the prepared composite is unstable.
Disclosure of Invention
The invention aims to provide a preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material, which has the advantages of simple process, short molding time and low cost, and can effectively increase the interfacial bonding strength of carbon fibers and quartz ceramic matrixes and the bending strength perpendicular to the fiber direction in the prepared composite material, and the prepared composite material has good high-temperature stability and self-healing performance.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material comprises the following steps:
(1) Pretreatment of continuous carbon fiber: soaking the continuous carbon fiber in acetone, then washing with distilled water for 3-5 times, and then drying in an oven for the first time; immersing the dried continuous carbon fiber into pure methanol completely, stirring ultrasonically, separating the continuous carbon fiber from the solution, and drying in an oven for the second time until the continuous carbon fiber is dried completely;
(2) Preparing a dipping material: adding fused quartz powder, zirconia powder and grinding balls into a ball milling tank, adding a dispersing agent, mixing in ionized water, and performing ball milling to obtain an impregnating material;
(3) And (3) dip molding: impregnating the pretreated continuous carbon fibers in the step (1) into the impregnating material prepared in the step (2), carrying out vibration impregnation treatment under vacuum conditions, drying to constant weight after impregnation, putting the impregnated material into the impregnating material again for 3-5 times, and drying to constant weight after impregnation is completed to obtain the impregnated and molded composite material;
(4) And (3) drying and sintering: and drying the composite material after the dip molding, stacking in a graphite mold, and hot-pressing and sintering under nitrogen atmosphere to obtain the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material.
Preferably, in the step (1), the mass ratio between the continuous carbon fiber and the pure methanol is 1 (3-5).
Preferably, in the step (1), the continuous carbon fiber is soaked in the acetone for 12-20 hours; the ultrasonic stirring time is 20-40min.
Preferably, in step (1), the first drying process parameters are: the drying temperature is 70-80 ℃ and the drying time is 12-18h; the second drying temperature is 80-90 ℃.
Preferably, in the step (2), one or more of isopropanol, ammonium citrate and lactic acid serving as dispersing agents are added in an amount of 1-3% of the total mass of the fused quartz powder and the zirconia powder.
Preferably, in the step (2), the average particle sizes of the fused quartz powder and the zirconia powder are respectively 5-8 μm and 0.5-1 μm; the grinding balls are agate balls or zirconia balls; the rotating speed of the ball mill is 15-25r/min, and the ball milling time is 16-24h.
Preferably, in the step (3), the vacuum degree is-0.08 to-0.05 MPa; the vibration time is 4-6min per vibration, and the interval is 3-4min; the soaking time is 30-40min; the content of the continuous carbon fiber in the composite material after the dip molding is 20-35vol.%.
Preferably, in the step (4), the nitrogen addition rate is 200-260cc/min; the sintering temperature is 1200-1300 ℃ and the pressure is 15-18MPa.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention adopts submicron zirconia particles to modify the anisotropy of the continuous carbon fiber reinforced silica composite material, and the dispersion of zirconia enhances the interfacial sliding stress on the interface of the carbon fiber and the quartz ceramic matrix, thereby effectively increasing the interfacial bonding strength of the carbon fiber and the quartz ceramic matrix and the bending resistance perpendicular to the fiber direction.
2. The invention adopts hot-pressing sintering, thereby improving the molding rate of the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material, having good high-temperature stability and self-healing property, and preparing composite materials with different densities under the condition of little change of bending strength by adjusting the proportion of different additives, so as to realize high-performance light refractory materials.
3. The preparation method has the advantages of simple preparation process, short molding time and low cost, and the prepared composite material can be used for molding mechanical components only by a small amount of processing or no processing.
Drawings
FIG. 1 is a transmission electron microscope image of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material prepared in example 1 of the present invention.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
Example 1
A preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material comprises the following steps:
(1) Pretreatment of continuous carbon fiber: soaking the continuous carbon fiber in acetone for 12 hours, washing with distilled water for 3 times, and then drying in an oven at 80 ℃ for 12 hours; immersing the dried continuous carbon fiber into pure methanol completely, wherein the mass ratio of the continuous carbon fiber to the pure methanol is 1:5, carrying out ultrasonic stirring, separating the continuous carbon fiber from the solution, and putting the solution into an oven at 80 ℃ until the solution is completely dried;
(2) Preparing a dipping material: adding fused quartz powder, zirconia powder and agate balls with average particle diameters of 8 mu m and 0.5 mu m into a ball milling tank, adding dispersant isopropanol accounting for 1% of the total mass of the fused quartz powder and the zirconia powder, mixing in ionized water, and carrying out ball milling at the rotating speed of 15r/min for 24 hours to obtain an impregnating compound;
(3) And (3) dip molding: impregnating the pretreated continuous carbon fibers in the step (1) into the impregnating compound prepared in the step (2), carrying out vibration impregnation treatment under the conditions of a vacuum degree of-0.05 MPa, an auxiliary vibration time of 4min per vibration and an intermittent vibration time of 4min, wherein the impregnation time is 30min, drying the impregnated continuous carbon fibers to constant weight, putting the impregnated continuous carbon fibers into the impregnating compound again for 3 times, and drying the impregnated continuous carbon fibers to constant weight to obtain an impregnated composite material, wherein the content of the continuous carbon fibers in the composite material is 35 vol%;
(4) And (3) drying and sintering: stacking the composite material subjected to dip molding in a graphite mold, wherein the adding speed of nitrogen is 200cc/min; and hot-pressing and sintering at 1200 ℃ and 15MPa to obtain the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material, and respectively performing bending strength tests on the composite material in a direction parallel to the fiber direction and a direction perpendicular to the fiber direction, wherein the test results are shown in the following table 1.
Fig. 1 is a transmission electron microscope image of the composite material prepared in example 1 of the present invention, and it can be seen from the image that a zirconia layer is distributed between the carbon fiber and the quartz substrate, and the carbon fiber and the quartz substrate are well combined.
Example 2
A preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material comprises the following steps:
(1) Pretreatment of continuous carbon fiber: soaking the continuous carbon fiber in acetone for 18h, washing with distilled water for 5 times, and then drying in an oven at 70 ℃ for 18h; then, completely immersing the dried continuous carbon fiber into pure methanol, wherein the mass ratio of the continuous carbon fiber to the pure methanol is 1:3, ultrasonically stirring, separating the continuous carbon fiber from the solution, and putting the solution into a baking oven at 90 ℃ until the solution is completely dried;
(2) Preparing a dipping material: adding fused quartz powder, zirconia powder and zirconia balls with average particle diameters of 5 mu m and 1 mu m into a ball milling tank, adding ammonium citrate serving as a dispersing agent and accounting for 2% of the total mass of the fused quartz powder and the zirconia powder, mixing in ionized water, and performing ball milling at the rotating speed of 20r/min for 18 hours to obtain an impregnating material;
(3) And (3) dip molding: impregnating the pretreated continuous carbon fibers in the step (1) into the impregnating compound prepared in the step (2), carrying out vibration impregnation treatment under the conditions of vacuum degree of-0.075 Mpa, auxiliary vibration time of 5min per vibration and intermittent 4min, wherein the impregnation time is 40min, drying to constant weight after impregnation, putting the impregnated material into the impregnating compound again for circulation for 3 times, and drying to constant weight after impregnation is finished to obtain an impregnated composite material, wherein the content of the continuous carbon fibers in the composite material is 30 vol%;
(4) And (3) drying and sintering: stacking the composite material subjected to dip molding in a graphite mold, wherein the adding speed of nitrogen is 260cc/min; sintering at 1280 ℃ and 18MPa to obtain the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material, and respectively performing bending strength tests on the composite material in a direction parallel to the fiber direction and a direction perpendicular to the fiber direction, wherein the test results are shown in the following table 1.
Example 3
A preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material comprises the following steps:
(1) Pretreatment of continuous carbon fiber: soaking the continuous carbon fiber in acetone for 20h, washing with distilled water for 5 times, and drying in an oven at 80 ℃ for 12h; then, completely immersing the dried continuous carbon fiber into pure methanol, wherein the mass ratio of the continuous carbon fiber to the pure methanol is 1:4, carrying out ultrasonic stirring, separating the continuous carbon fiber from the solution, and putting the solution into a baking oven at 90 ℃ until the solution is completely dried;
(2) Preparing a dipping material: adding fused quartz powder, zirconia powder, agate balls and zirconia balls with average particle diameters of 3 mu m and 0.8 mu m into a ball milling tank, adding dispersant lactic acid accounting for 3% of the total mass of the fused quartz powder and the zirconia powder, mixing in ionized water, and carrying out ball milling at the rotating speed of 25r/min for 18h to obtain an impregnating material;
(3) And (3) dip molding: impregnating the pretreated continuous carbon fibers in the step (1) into the impregnating compound prepared in the step (2), carrying out vibration impregnation treatment under the conditions of a vacuum degree of-0.05 Mpa, an auxiliary vibration time of 4min per vibration and an intermittent vibration time of 4min, wherein the impregnation time is 30min, drying to constant weight after impregnation is finished to obtain an impregnated composite material, and putting the impregnated composite material into the impregnating compound again for 3 times for circulation, wherein the content of the continuous carbon fibers in the composite material is 25 vol%;
(4) And (3) drying and sintering: stacking the composite material subjected to dip molding in a graphite mold, wherein the adding speed of nitrogen is 200cc/min; and hot-pressing and sintering at 1300 ℃ and 15MPa to obtain the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material, and respectively performing bending strength tests on the composite material in a direction parallel to the fiber direction and a direction perpendicular to the fiber direction, wherein the test results are shown in the following table 1.
Example 4
A preparation method of a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material comprises the following steps:
(1) Pretreatment of continuous carbon fiber: soaking the continuous carbon fiber in acetone for 16 hours, washing the continuous carbon fiber with distilled water for 4 times, and then drying the continuous carbon fiber in an oven at 70 ℃ for 16 hours; then, completely immersing the dried continuous carbon fiber into pure methanol, wherein the mass ratio of the continuous carbon fiber to the pure methanol is 1:4.5, carrying out ultrasonic stirring, separating the continuous carbon fiber from the solution, and putting the solution into a baking oven at 90 ℃ until the solution is completely dried;
(2) Preparing a dipping material: adding fused quartz powder, zirconia powder and zirconia balls with average particle diameters of 8 mu m and 0.8 mu m into a ball milling tank, adding dispersant isopropanol and ammonium citrate which are 1.5% of the total mass of the fused quartz powder and the zirconia powder, mixing in ionized water, and carrying out ball milling at the rotating speed of 25r/min for 16 hours to obtain an impregnating material;
(3) And (3) dip molding: impregnating the pretreated continuous carbon fibers in the step (1) into the impregnating compound prepared in the step (2), carrying out vibration impregnation treatment under the conditions of a vacuum degree of-0.08 Mpa, an auxiliary vibration time of 6min per vibration and an intermittent vibration time of 3min, wherein the impregnation time is 40min, drying to constant weight after impregnation is finished to obtain an impregnated composite material, and putting the impregnated composite material into the impregnating compound again for 3 times for circulation, wherein the content of the continuous carbon fibers in the composite material is 20 vol%;
(4) And (3) drying and sintering: stacking the composite material subjected to dip molding in a graphite mold, wherein the adding speed of nitrogen is 200cc/min; sintering at 1220 ℃ and 17MPa to obtain the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material, and respectively performing bending strength tests on the composite material in a direction parallel to the fiber direction and a direction perpendicular to the fiber direction, wherein the test results are shown in the following table 1.
Table 1 results of performance testing of samples prepared in examples
As can be seen from Table 1, the density of the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material prepared by the invention is high, the bending strength parallel to the fiber direction is greater than 530MPa, and most importantly, the bending strength perpendicular to the fiber direction is greater than 50MPa, and the strength improvement is obvious. Therefore, the composite material prepared by the invention has high density and high strength, and especially has bending strength perpendicular to the fiber direction.

Claims (8)

1. The preparation method of the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material is characterized by comprising the following steps of:
(1) Pretreatment of continuous carbon fiber: soaking the continuous carbon fiber in acetone, then washing with distilled water for 3-5 times, and then drying in an oven for the first time; immersing the dried continuous carbon fiber into pure methanol completely, stirring ultrasonically, separating the continuous carbon fiber from the solution, and drying in an oven for the second time until the continuous carbon fiber is dried completely;
(2) Preparing a dipping material: adding fused quartz powder, zirconia powder and grinding balls into a ball milling tank, adding a dispersing agent, mixing in ionized water, and performing ball milling to obtain an impregnating material;
(3) And (3) dip molding: impregnating the pretreated continuous carbon fibers in the step (1) into the impregnating material prepared in the step (2), carrying out vibration impregnation treatment under vacuum conditions, drying to constant weight after impregnation, putting the impregnated material into the impregnating material again for 3-5 times, and drying to constant weight after impregnation is completed to obtain the impregnated and molded composite material;
(4) And (3) drying and sintering: stacking the composite material after the dip molding in a graphite mold, and hot-pressing and sintering the composite material in a nitrogen atmosphere to obtain the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material.
2. The zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material and the preparation method thereof according to claim 1, wherein in the step (1), the mass ratio of the continuous carbon fiber to the pure methanol is 1 (3-5).
3. The zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material and the preparation method thereof according to claim 1 or 2, wherein in the step (1), the soaking time of the continuous carbon fiber in acetone is 12-20h; the ultrasonic stirring time is 20-40min.
4. The zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material and the preparation method thereof according to claim 1 or 2, wherein in the step (1), the first drying process parameters are as follows: the drying temperature is 70-80 ℃ and the drying time is 12-18h; the second drying temperature is 80-90 ℃.
5. The method for preparing the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material according to claim 1 or 2, wherein in the step (2), one or more of isopropanol, ammonium citrate and lactic acid serving as a dispersing agent is added in an amount of 1-3% of the total mass of the fused quartz powder and the zirconia powder.
6. The method for preparing a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material according to claim 1 or 2, wherein in the step (2), the average particle diameters of the fused quartz powder and the zirconia powder are 5-8 μm and 0.5-1 μm, respectively; the grinding balls are agate balls or zirconia balls; the rotating speed of the ball mill is 15-25r/min, and the ball milling time is 16-24h.
7. The method for preparing the zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material according to claim 1 or 2, wherein in the step (3), the vacuum degree is-0.08 to-0.05 MPa; the vibration time is 4-6min per vibration, and the interval is 3-4min; the soaking time is 30-40min; the content of the continuous carbon fiber in the composite material after the dip molding is 20-35vol.%.
8. The method for producing a zirconia and continuous carbon fiber co-reinforced quartz ceramic composite according to claim 1 or 2, wherein in the step (4), the nitrogen addition rate is 200-260cc/min; the sintering temperature is 1200-1300 ℃ and the pressure is 15-18MPa.
CN202311735496.2A 2023-12-15 2023-12-15 Preparation method of zirconia and continuous carbon fiber co-reinforced quartz ceramic composite material Pending CN117865660A (en)

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