CN112299854A - Low-cost high-temperature-resistant carbon-ceramic composite material and preparation method thereof - Google Patents
Low-cost high-temperature-resistant carbon-ceramic composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low-cost high-temperature-resistant carbon-ceramic composite material and a preparation method thereof. The method comprises the steps of uniformly inserting a multi-needle injector filled with a precursor on the surface of a carbon-ceramic composite material reinforcement, symmetrically arranging the multi-needle injector and the carbon-ceramic composite material reinforcement around a centrifugal cylinder, starting the centrifugal cylinder, uniformly penetrating the precursor in the multi-needle injector into the lower surface of the carbon-ceramic composite material reinforcement from the upper surface of the carbon-ceramic composite material reinforcement under the action of centrifugal force, volatilizing moisture of the multi-needle injector under the action of heating, reserving solid content in the carbon-ceramic composite material reinforcement to form a densified and dried carbon-ceramic composite material green body base body, and sintering to obtain the carbon-ceramic composite material. The carbon-ceramic composite material is high temperature resistant and low in preparation cost.
Description
Technical Field
The invention relates to a low-cost high-temperature-resistant carbon-ceramic composite material and a preparation method thereof, belonging to the technical field of carbon-ceramic composite materials.
Background
The carbon-ceramic composite material is a novel high-temperature-resistant oxidation-resistant ceramic matrix composite material developed following a carbon-carbon composite material, and the design target of the carbon-ceramic composite material is that the carbon-ceramic composite material has more excellent high-temperature oxidation resistance, high-temperature water vapor corrosion resistance and friction performance than the carbon-carbon composite material. Therefore, the composite material has great application value in the aspects of new-generation high-performance airplane friction materials and high-temperature ablation-resistant materials, and is a novel ceramic matrix composite material which is competitively researched in developed countries such as Europe and America.
The traditional preparation methods of the ceramic composite materials mainly comprise two main types: firstly, a carbon fiber or silicon carbide fiber reinforcement is adopted to impregnate an organic precursor melt or solution containing elements such as carbon, silicon, oxygen and the like through a multiple impregnation cracking route, and then the carbon fiber reinforced silicon carbide composite material is prepared through high-temperature oxygen-free or inert gas protection cracking. Because the porosity of the carbon-ceramic composite material obtained by one-time impregnation and cracking is higher, in order to improve the density, multiple times of impregnation and cracking are needed. Meanwhile, the organic precursor containing carbon, silicon, oxygen and other elements has high cost due to the great difficulty of the synthesis technology. Therefore, the process has high energy consumption and long preparation period, and leads to extremely high cost of the carbon-ceramic composite material. The other method is to adopt a chemical vapor infiltration route of a gaseous precursor containing elements such as carbon, silicon and the like in a carbon fiber or silicon carbide fiber reinforcement to crack the gaseous precursor containing the elements such as carbon, silicon and the like at high temperature to obtain the carbon-ceramic composite material with high density. The method can obtain the ceramic matrix composite material with high density due to gas permeation, but the common industrial method has extremely high energy consumption cost and time cost due to low vapor infiltration deposition efficiency.
Therefore, in order to expand the application field of the carbon-ceramic composite material and reduce the preparation cost, a low-cost precursor and a preparation process method are urgently needed to be developed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the low-cost high-temperature-resistant carbon ceramic composite material and the preparation method thereof.
The technical scheme for solving the technical problems is as follows: a low-cost high-temperature-resistant carbon-ceramic composite material is obtained by densifying a carbon-ceramic composite material reinforcement by using a precursor, wherein the precursor comprises tetraethoxysilane, aluminum powder, absolute ethyl alcohol, trimethyldichlorosilane and alkaline silica sol, and the synthesis process of the precursor is as follows:
1) uniformly mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water at room temperature to prepare a solution containing silicon and an oxygen source;
2) under the condition of air isolation, slowly dripping trimethyldichlorosilane into the aluminum powder, and slowly stirring;
3) slowly dropwise adding alkaline silica sol into the mixture of the aluminum powder and the methyl dichlorosilane in the step 2), adjusting the pH value to 9-10.5 by using ammonia water, and forming colloid on the aluminum powder at the temperature of 60-95 ℃ to obtain colloid aluminum powder;
4) uniformly mixing the solution containing silicon and oxygen in the step 1) with the colloidal aluminum powder in the step 3), stirring, and adding deionized water to adjust the viscosity to be 100-800cps to obtain a precursor.
Preferably, in the step 1), the molar ratio of the ethyl orthosilicate to the absolute ethyl alcohol to the deionized water is 1: 0.65-2.5: 1.2-2.8.
Preferably, in the step 2), the molar ratio of the aluminum powder to the trimethyldichlorosilane is 1: 0.05 to 0.08, and the aluminum powder is 80 to 120 meshes of spherical aluminum powder.
Preferably, in the step 4), the mass ratio of the solution containing silicon and an oxygen source to the colloidal aluminum powder is 1: 0.7 to 1.5.
The invention also discloses a preparation method of the low-cost high-temperature-resistant carbon ceramic composite material, which comprises the following steps:
(a) cutting a commercial carbon fiber or silicon carbide fiber preformed body into regular blocks serving as a carbon ceramic composite material reinforcement;
(b) placing the precursor in a multi-needle injector for injecting and densifying the carbon-ceramic composite material reinforcement;
(c) symmetrically placing the carbon-ceramic composite material reinforcement in a centrifugal cylinder rotating at a high speed, introducing heat conduction oil or steam between the inner wall of the centrifugal cylinder and the outer wall of the centrifugal cylinder, heating a commercial carbon fiber or silicon carbide fiber preform, evaporating water in a precursor, and embedding a high-speed bearing in a central shaft of the centrifugal cylinder;
(d) uniformly inserting a multi-needle syringe filled with a precursor on the surface of a carbon-ceramic composite material reinforcement, symmetrically arranging the multi-needle syringe and the carbon-ceramic composite material reinforcement around a centrifuge cylinder, and clamping and fixing;
(e) starting the centrifugal cylinder, starting a heating function of heat conduction oil or steam between the inner wall of the centrifugal cylinder and the outer wall of the centrifugal cylinder, enabling a precursor in the multi-needle injector to uniformly permeate into the lower surface from the upper surface of the carbon-ceramic composite material reinforcement under the action of centrifugal force, enabling the multi-driver to volatilize water under the gradient heating action of the inner wall of the centrifugal cylinder, and retaining solid content in the carbon-ceramic composite material reinforcement to form a densified and dried carbon-ceramic composite material green body;
(f) and (e) placing the carbon-ceramic composite material green body substrate obtained in the step (e) into an atmosphere protection furnace or a vacuum furnace for sintering to obtain the carbon-ceramic composite material.
Further, the inner wall of the centrifugal cylinder is coated with a heating body with high emissivity, and the inner wall of the centrifugal cylinder is coated with a carbon black or graphite coating; and a heat insulation material is arranged outside the outer wall of the centrifugal cylinder.
Further, in the step (e), the rotation speed of the centrifugal cylinder is 500-.
Further, in the step (f), the sintering temperature is 1400 ℃ 1850 ℃.
The invention has the beneficial effects that: the carbon-ceramic composite material has a smooth surface, no obvious air holes or deformation, a compact overall structure, a compactness of more than 95%, and a bending strength of 220MPa at most and 98MPa at least. The carbon-ceramic composite material is high-temperature resistant, low in preparation cost and suitable for industrial production.
Drawings
FIG. 1 is a schematic view of a centrifuge tube with heating function;
FIG. 2 is an optical photograph of the carbon ceramic composite material prepared in the example;
FIG. 3 is an SEM microtopography of the surface of the carbon ceramic composite material prepared in the example (a) low-power (b) high-power sheet;
in the figure, a 1 carbon ceramic composite material reinforcement body; 2. the inner wall of the centrifugal cylinder; 3, centrifuging the outer wall of the cylinder; 4, a multi-needle injector; 5. a central axis.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
A low-cost high-temperature-resistant carbon-ceramic composite material is obtained by densifying a carbon-ceramic composite material reinforcement 1 by using a precursor, wherein the precursor comprises tetraethoxysilane, aluminum powder, absolute ethyl alcohol, trimethyldichlorosilane and alkaline silica sol, and the synthesis process of the precursor is as follows:
1) ethyl orthosilicate, absolute ethyl alcohol and deionized water are mixed according to a molar ratio of 1: 0.65-2.5: 1.2-2.8, and uniformly mixing at room temperature to prepare a solution containing silicon and an oxygen source;
2) under the condition of air isolation, slowly dropwise adding trimethyldichlorosilane into aluminum powder, and slowly stirring, wherein the molar ratio of the aluminum powder to the trimethyldichlorosilane is 1: 0.05 to 0.08, wherein the aluminum powder is spherical aluminum powder with 80 to 120 meshes;
3) slowly dropwise adding alkaline silica sol into the mixture of the aluminum powder and the methyl dichlorosilane in the step 2), adjusting the pH value to 9-10.5 by using ammonia water, and forming colloid on the aluminum powder at the temperature of 60-95 ℃ to obtain colloid aluminum powder;
4) mixing the solution containing silicon and oxygen source in the step 1) and the colloidal aluminum powder in the step 3) according to the mass ratio of 1: 0.7-1.5, stirring, adding deionized water to adjust the viscosity to 100-800cps, and obtaining the precursor.
The preparation method of the low-cost high-temperature-resistant carbon-ceramic composite material comprises the following steps:
(a) cutting a commercial carbon fiber or silicon carbide fiber preformed body into regular blocks serving as a carbon ceramic composite material reinforcement 1;
(b) placing the precursor in a multi-needle injector 4 for injecting and densifying the carbon-ceramic composite material reinforcement 1;
(c) the carbon-ceramic composite material reinforcement 1 is symmetrically arranged in a centrifugal cylinder rotating at a high speed, heat conducting oil or steam is introduced between the inner wall 2 of the centrifugal cylinder and the outer wall 3 of the centrifugal cylinder, a high-speed bearing is embedded in a central shaft 5 of the centrifugal cylinder, the inner wall 2 of the centrifugal cylinder is coated with a heating body with high emissivity, the inner wall 2 of the centrifugal cylinder is coated with carbon black or a graphite coating, and a heat insulation material is arranged outside the outer wall 3 of the centrifugal cylinder. (ii) a
(d) Uniformly inserting a multi-needle syringe 4 filled with a precursor on the surface of a carbon-ceramic composite material reinforcement 1, symmetrically arranging the multi-needle syringe 4 and the carbon-ceramic composite material reinforcement 1 around a centrifuge cylinder, and clamping and fixing;
(e) starting a centrifugal cylinder, wherein the rotation speed of the centrifugal cylinder is 500-8000rpm, starting the heating function of heat conduction oil or steam between the inner wall 2 of the centrifugal cylinder and the outer wall 3 of the centrifugal cylinder, the heating temperature is 90-200 ℃, a precursor in a multi-needle injector 4 uniformly permeates into the lower surface from the upper surface of a carbon-ceramic composite material reinforcement body 1 under the action of centrifugal force, the multi-drive body volatilizes water under the gradient heating action of the inner wall 2 of the centrifugal cylinder, and the solid content is remained in the carbon-ceramic composite material reinforcement body 1 to form a densified and dried carbon-ceramic composite material green body matrix, and the centrifugation time is 2-30 h;
(f) and (e) placing the green substrate of the carbon-ceramic composite material obtained in the step (e) in an atmosphere protection furnace or a vacuum furnace for sintering at the sintering temperature of 1400 ℃ and 1850 ℃ to obtain the carbon-ceramic composite material.
The optical photo of the carbon-ceramic composite material shows that the surface is relatively flat after sintering, and no obvious air holes or deformation exists.
As can be seen from the SEM microscopic morphology picture of the surface of the carbon ceramic composite material, the whole structure is compact, micropores are randomly distributed in the microscopic view, and the diameter of each micropore is about 100-400nm according to the scanning picture result. The density is more than 95% according to a drainage method. According to a three-point bending test, the bending strength of the prepared carbon-ceramic composite material can reach 220MPa at most and 98MPa at least.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (8)
1. The low-cost high-temperature-resistant carbon-ceramic composite material is characterized in that the carbon-ceramic composite material is obtained by densifying a carbon-ceramic composite material reinforcement by using a precursor, the precursor raw materials comprise tetraethoxysilane, aluminum powder, absolute ethyl alcohol, trimethyldichlorosilane and alkaline silica sol, and the synthesis process of the precursor is as follows:
1) uniformly mixing ethyl orthosilicate, absolute ethyl alcohol and deionized water at room temperature to prepare a solution containing silicon and an oxygen source;
2) under the condition of air isolation, slowly dripping trimethyldichlorosilane into the aluminum powder, and slowly stirring;
3) slowly dropwise adding alkaline silica sol into the mixture of the aluminum powder and the methyl dichlorosilane in the step 2), adjusting the pH value to 9-10.5 by using ammonia water, and forming colloid on the aluminum powder at the temperature of 60-95 ℃ to obtain colloid aluminum powder;
4) uniformly mixing the solution containing silicon and oxygen in the step 1) with the colloidal aluminum powder in the step 3), stirring, and adding deionized water to adjust the viscosity to be 100-800cps to obtain a precursor.
2. The low-cost high-temperature-resistant carbon-ceramic composite material as claimed in claim 1, wherein in the step 1), the molar ratio of the tetraethoxysilane to the absolute ethyl alcohol to the deionized water is 1: 0.65-2.5: 1.2-2.8.
3. The low-cost high-temperature-resistant carbon-ceramic composite material as claimed in claim 1, wherein in the step 2), the molar ratio of the aluminum powder to the trimethyldichlorosilane is 1: 0.05 to 0.08, and the aluminum powder is 80 to 120 meshes of spherical aluminum powder.
4. The low-cost high-temperature-resistant carbon-ceramic composite material as claimed in claim 1, wherein in the step 4), the mass ratio of the solution containing silicon and oxygen source to the colloidal aluminum powder is 1: 0.7 to 1.5.
5. A preparation method of the low-cost high-temperature-resistant carbon-ceramic composite material according to any one of claims 1 to 4, characterized by comprising the following steps of:
(a) cutting a commercial carbon fiber or silicon carbide fiber preformed body into regular blocks serving as a carbon ceramic composite material reinforcement;
(b) placing the precursor in a multi-needle injector for injecting and densifying the carbon-ceramic composite material reinforcement;
(c) symmetrically placing the carbon-ceramic composite material reinforcement in a centrifugal cylinder rotating at a high speed, introducing heat conduction oil or steam between the inner wall of the centrifugal cylinder and the outer wall of the centrifugal cylinder, and embedding a high-speed bearing in a central shaft of the centrifugal cylinder;
(d) uniformly inserting a multi-needle syringe filled with a precursor on the surface of a carbon-ceramic composite material reinforcement, symmetrically arranging the multi-needle syringe and the carbon-ceramic composite material reinforcement around a centrifuge cylinder, and clamping and fixing;
(e) starting the centrifugal cylinder, starting a heating function of heat conduction oil or steam between the inner wall of the centrifugal cylinder and the outer wall of the centrifugal cylinder, enabling a precursor in the multi-needle injector to uniformly permeate into the lower surface from the upper surface of the carbon-ceramic composite material reinforcement under the action of centrifugal force, enabling the multi-driver to volatilize water under the gradient heating action of the inner wall of the centrifugal cylinder, and retaining solid content in the carbon-ceramic composite material reinforcement to form a densified and dried carbon-ceramic composite material green body;
(f) and (e) placing the carbon-ceramic composite material green body substrate obtained in the step (e) into an atmosphere protection furnace or a vacuum furnace for sintering to obtain the carbon-ceramic composite material.
6. The preparation method of the low-cost high-temperature-resistant carbon-ceramic composite material as claimed in claim 5, wherein the inner wall of the centrifugal cylinder is coated with a high-emissivity heating body, and the inner wall of the centrifugal cylinder is coated with a carbon black or graphite coating; and a heat insulation material is arranged outside the outer wall of the centrifugal cylinder.
7. The method as claimed in claim 5, wherein in the step (e), the rotation speed of the centrifuge cylinder is 500-.
8. The method as claimed in claim 5, wherein the sintering temperature in step (f) is 1400-1850 ℃.
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| CN109825903A (en) * | 2019-03-04 | 2019-05-31 | 中国科学院宁波材料技术与工程研究所 | A kind of aluminum-containing silicon carbide fiber and preparation method thereof |
| CN110713385A (en) * | 2019-11-28 | 2020-01-21 | 湖南博云新材料股份有限公司 | Preparation method of carbon-ceramic friction material |
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