CN111377750A - Carbon nanotube sponge reinforced silicon carbide ceramic matrix composite and preparation method thereof - Google Patents
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Abstract
The invention relates to a carbon nanotube sponge reinforced silicon carbide ceramic matrix composite and a preparation method thereof, wherein the preparation method of the carbon nanotube sponge reinforced silicon carbide ceramic matrix composite comprises the following steps: selecting carbon nanotube sponge as a prefabricated body, Ar as a carrier gas, and diluting with a diluent gas H2And introducing trichloromethyl silane MTS into a reaction furnace, heating to 800-1000 ℃, and starting to deposit SiC to obtain the carbon nanotube sponge reinforced silicon carbide ceramic matrix composite.
Description
Technical Field
The invention relates to a carbon nanotube sponge reinforced silicon carbide ceramic matrix composite and a preparation method thereof, belonging to the field of composite preparation.
Background
In ceramic matrix composite materials, silicon carbide (SiC) ceramic materials are regarded as important due to their superior properties such as high hardness, low expansion coefficient, high thermal conductivity, high acid and alkali resistance, and exhibit incomparable application space in the aspects of machinery, aerospace, military industry and the like, but the application is limited by the influence of the characteristics of the ceramic materials, such as brittleness, electrical conductivity, thermal conductivity and the like. Therefore, the properties of the silicon carbide ceramic material are improved, and the wider application of the silicon carbide ceramic material can be expanded.
The carbon nano tube reinforcement can make up the defect of the characteristic of the silicon carbide ceramic material and improve the performance of the silicon carbide ceramic material. However, the dispersion of carbon nanotubes in the matrix has been an urgent problem to be solved. The agglomeration of the carbon nanotubes prevents the formation of ideal mutual combination between the carbon nanotube monomer and the matrix, which can seriously affect the combination of the interface and the microstructure, and finally leads to the damage of the physical and chemical properties of the composite material.
Disclosure of Invention
The invention provides a carbon nanotube sponge reinforced silicon carbide ceramic matrix composite and a preparation method thereof, aiming at the problems that the silicon carbide ceramic matrix in the existing carbon nanotube reinforced silicon carbide ceramic composite is heavy in weight, poor in performances of electric conduction, heat conduction and the like, carbon nanotubes are agglomerated in the ceramic matrix, and the composite strength of a carbon nanotube sponge reinforcement and a matrix material is low and easy to damage.
On one hand, the invention provides a preparation method of a carbon nanotube sponge reinforced silicon carbide ceramic matrix composite, which selects carbon nanotube sponge as a prefabricated body, uses Ar as a carrier gas, and uses a diluent gas H2And introducing the trichloromethylsilane MTS and the MTS into a reaction furnace, heating to 800-1000 ℃, and starting to deposit SiC to obtain the carbon nanotube sponge reinforced silicon carbide ceramic matrix composite.
In this disclosure, trichloromethylsilane (MTS) is used with H using Chemical Vapor Infiltration (CVI)2Delivering the carbon nano tube to the surface of the carbon nano tube sponge with porous pores, carrying out chemical reaction on the carbon nano tube sponge to generate silicon carbide and depositing the silicon carbide to form a silicon carbide ceramic matrix, and forming the silicon carbide ceramic matrix composite together with the carbon nano tube sponge. During deposition of SiC, gaseous by-products are exhausted through the porous spaces of the carbon nanotube sponge with the carrier gas. Moreover, the densified composite material obtained by using the carbon nanotube sponge to carry out the chemical vapor infiltration method can avoid the agglomeration of the carbon nanotubes and the damage of the structure of the carbon nanotube sponge reinforcement body by high temperature and high pressure. In addition, the composite material with incomplete compactness and lighter weight can be prepared by adopting a chemical vapor infiltration method according to the regulation and control of the deposition time.
Preferably, the diluent gas H2The flow rate of (1) is 1500-2000 sccm; the MTS of the trichloromethyl silicon is 150-200 sccm; the flow rate of the argon is 4500-6000 sccm.
Preferably, the diluentGas H2And trichloromethyl silicone MTS in a volume ratio of (10-11): 1.
preferably, the pressure in the reaction furnace is 9-12 KPa.
Preferably, the deposition time is 200 to 600 hours.
Preferably, the temperature rise rate is 3-7 ℃/min.
Preferably, the preparation method of the carbon nanotube sponge comprises the following steps:
mixing a catalyst, an accelerant and a liquid carbon source to obtain a precursor solution;
introducing a mixed gas of argon and hydrogen into a reaction furnace, heating to 1000-1300 ℃, and injecting a precursor solution into the reaction furnace to start the growth of the carbon nano tube;
the obtained carbon nano tube is deposited on a scroll along with carrier gas flow to obtain carbon nano tube sponge;
the catalyst is at least one of ferrocene, cobaltocene and nickelocene; the accelerant is thiophene; the liquid carbon source is at least one of absolute ethyl alcohol, methanol and diethyl ether. The carbon nanotube sponge prepared by the method is an ultra-light 3D structural material and has excellent performances of low density, multiple pores, high conductivity, high strength, high surface area and low atomic weight.
Preferably, the concentration of the catalyst in the precursor solution is 1 to 3 wt%, and the concentration of the accelerator is 0.5 to 1 wt%.
In addition, preferably, the injection rate of the precursor solution is 18-22 mL/h; the rotating speed of the reel is 4-6 m/min.
In addition, in the preparation method of the carbon nanotube sponge, the flow rate of argon is 1800-2200 sccm, and the flow rate of hydrogen is 1600-2000 sccm.
In addition, the temperature of the needle or the nozzle used for injecting the precursor solution is preferably between 500 ℃ and 550 ℃, so that the carbon nanotube with the optimal quality is obtained and is beneficial to being deposited on the reel to form the carbon nanotube sponge.
In another aspect, the present invention provides a carbon nanotube sponge-reinforced silicon carbide ceramic matrix composite prepared according to the above preparation method. The carbon nanotube sponge reinforced silicon carbide ceramic matrix composite material is a novel ceramic matrix composite functional material with high electrical conductivity, high thermal conductivity and high hemispherical emissivity under the condition of low density, and has wide application prospects in the application fields of electromagnetic shielding, stealth, thermal management and the like.
Has the advantages that:
the reinforcement provided by the invention is the carbon nanotube sponge, and the density of the obtained silicon carbide ceramic matrix composite material is lower than that of the carbon fiber reinforced silicon carbide ceramic matrix composite material;
the silicon carbide ceramic matrix composite material prepared by the invention has the properties of lighter weight, higher electrical conductivity, higher thermal conductivity and higher hemispherical total emissivity;
the carbon nanotube sponge reinforcement used in the invention can avoid the key problems that the carbon nanotube is not easy to disperse and damage on the matrix and the bonding strength of the matrix is poor, and the directional performance difference is not easy to exist;
the chemical vapor infiltration process used by the invention can produce more light-weight incompletely compact composite material on the basis of not damaging the carbon nano tube sponge reinforcement;
the composite material provided by the invention has the advantages of simple integrated forming process and compact process, can meet the requirement of industrial production, and has wide application prospect in the application fields of electromagnetic shielding, stealth, thermal management and the like.
Drawings
FIG. 1 is a photograph of the composite material obtained in example 1;
FIG. 2 is a scanning electron microscope photograph of the composite material obtained in example 1-2;
FIG. 3 is an EDS diagram of the composite obtained in example 1;
FIG. 4 is a 3D confocal microscope photograph of the composite obtained in example 1.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the present disclosure, a method for preparing a carbon nanotube sponge reinforced silicon carbide ceramic matrix composite includes two parts: preparing a prefabricated carbon nanotube sponge and preparing a composite material.
And (3) preparing a prefabricated carbon nanotube sponge. Preparing carbon nanotubes by Chemical Vapor Deposition (CVD), and collecting to obtain carbon nanotube sponge.
Dissolving 2 wt% of ferrocene and 1 wt% of thiophene in absolute ethyl alcohol to prepare a precursor solution. Ar is introduced, and the temperature of the tube furnace is increased to 1280 ℃ at the speed of 10 ℃/min. The precursor solution is then pumped into a syringe pump, accompanied by Ar (e.g., 2000sccm) and H2(e.g., 1800sccm) was injected into the high temperature tube furnace at a rate of 21mL/h (needle temperature of about 520 ℃ C.). At this time, the tube furnace starts to produce continuous carbon nanotubes like a sock tube, and as the carrier gas flow flows out from the outlet of the furnace, a layer of carbon nanotube sponge is formed by wrapping the reel at the outlet. And the collected carbon nanotube sponge is used as single-layer carbon nanotube sponge after the reel rotates for one circle. The thickness of the obtained single-layer carbon nanotube sponge can be adjusted by adjusting the rotating speed of the reel, for example, the rotating speed can be 4-6 m/min, and the thickness of the corresponding single-layer carbon nanotube sponge can be 1-2 mm. By adjusting the collection time of the reel, the carbon nanotube sponge with a multilayer structure can be obtained. Preferably, the number of layers of the obtained carbon nanotube sponge can be 3-20. For example, the rotation speed of the reel is adjusted to 5m/min, and 3 layers (20min), 10 layers (1h) and 20 layers (2h) of carbon nanotube sponges are collected, respectively.
And preparing the carbon nanotube sponge reinforced silicon carbide ceramic matrix composite. Specifically, the carbon nanotube sponge is selected as a prefabricated body and prepared by using a Chemical Vapor Infiltration (CVI) method.
As an example, the carbon nanotube sponge is cut into 10 × 10cm size by a laser cutter, the carbon nanotube sponge with 3 thicknesses obtained above is placed in a soaking chamber of a furnace, the deposition furnace is washed by Ar, then the temperature is raised to 1000 ℃ at 5 ℃/min, H is introduced2Trichloromethylsilane (MTS, silicon carbide source) is introduced (as a diluent gas) into the reactor (H)2/MTS ═ 10), Ar as carrier gas, inThe deposition was carried out at a pressure of 10KPa in the furnace.
The gaseous MTS precursor diffuses and permeates into the pores of the carbon nanotube sponge and is adsorbed in the pores, SiC is generated by chemical reaction and deposited on the walls of the pores and is discharged into a lattice by surface diffusion, and the deposition time is hundreds of hours. As the deposition time increases, the pore wall surface gradually thickens and produces gaseous byproducts, which are desorbed from the pore wall and diffused in the carrier gas, and are discharged with Ar through the tail gas treatment. The invention is characterized in that the CNTs/SiC ceramic matrix composite is prepared by adopting carbon nanotube sponge as a prefabricated body and using a chemical vapor infiltration method, and a new material with wide application prospect in the application fields of electromagnetic shielding, stealth, thermal management and the like is obtained.
In the invention, the density of the obtained composite material is calculated by adopting the mass-to-volume ratio; testing the resistivity or conductivity of the obtained composite material by adopting a four-point method conductivity tester (RTS); testing the thermal diffusion coefficient and the thermal conductivity coefficient of the obtained composite material by adopting laser flash irradiation (LFA); and testing the hemispherical total emissivity of the obtained composite material by using a steady-state calorimeter method hemispherical total emissivity tester (the measurement temperature is 90 ℃).
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art in light of the foregoing description are intended to be included within the scope of the invention. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
(1) Preparing a precursor solution: dissolving ferrocene (2 wt%) and thiophene (1 wt%) in absolute ethyl alcohol, pumping into an injection pump, and obtaining a precursor solution;
(2) and (3) high-temperature reaction in a reaction furnace: ar is introduced, and the temperature of the tube furnace is increased to 1300 ℃ at the speed of 10 ℃/min. With Ar (2000sccm) and H2(1800sccm) of a mixed gas inInjecting the precursor solution in the injection pump into a high-temperature reaction furnace at the speed of 20mL/h at 1300 ℃, and starting the growth of the carbon nano tube when the temperature of a needle head is about 500 ℃;
(3) collecting the carbon nanotubes: installing a scroll at the outlet of the furnace (the rotation speed is 5m/min), and collecting for 20min to obtain 3 layers of carbon nanotube sponge (the thickness of a single layer is 2 mm);
(4) cutting the obtained carbon nanotube sponge (the length × is 10 × 10cm wide) by laser, and placing the carbon nanotube sponge in a soaking chamber;
(5) then the deposition furnace is flushed by Ar, the temperature is raised to 1000 ℃ at the speed of 5 ℃/min, and H is pumped in2Trichloromethylsilane (MTS) is introduced into a reaction furnace (H)2Volume ratio of MTS 10, H2The flow rate of (3) is 1500sccm), Ar is used as carrier gas (the flow rate is 4500sccm), and SiC deposition is carried out under the pressure of 10KPa in the furnace;
(6) after 250 hours of deposition, SiC was deposited on the pore wall surfaces of the carbon nanotube sponge and gaseous by-products were produced. The gaseous by-products are desorbed from the pore walls and diffused in the carrier gas, and are exhausted with the Ar through the tail gas treatment. Finally obtaining the densified carbon nanotube sponge reinforced silicon carbide ceramic matrix composite.
Example 2
The preparation method of the carbon nanotube sponge reinforced silicon carbide ceramic matrix composite in this example 2 includes all the steps in example 1, except that: in the step (3), the collection time of the carbon nano tubes is 1h, and 10 layers of carbon nano tube sponge is obtained; in step (6), the deposition was carried out for 310 hours.
Example 3
This example 3 illustrates a method for preparing a carbon nanotube sponge reinforced silicon carbide ceramic matrix composite, which includes all the steps of example 1, except that: in the step (3), the collection time of the carbon nano tubes is 2 hours, and 20 layers of carbon nano tube sponge is obtained; in step (6), the deposition was carried out for 360 hours.
Comparative example 1
The preparation method of the existing C/SiC ceramic matrix composite material comprises the following steps: the carbon fiber preform is a carbon fiber three-dimensional woven body formed by a weaving process and stacking, and the operation of step (5) is performed, and in step (6), the deposition is performed for 200 hours.
FIG. 1 is a static photograph of the composite material prepared in example 1, from which it can be seen that the CNTs/SiC ceramic matrix composite material is in the form of a black solid, hard, metallic luster, and substantially identical in shape to the carbon nanotube sponge preform;
FIG. 2 is a scanning electron microscope image of the composite materials prepared in example 1 and example 2, wherein (a), (c) are cross-sectional views of the 3-layer carbon nanotube sponge reinforced CNTs/SiC ceramic matrix composite material prepared in example 1 at different scales, respectively, (b), (d) are cross-sectional views of the carbon nanotube sponge reinforced CNTs/SiC ceramic matrix composite material prepared in example 2 at different scales, respectively, and (e) is a cross-sectional view of the composite material prepared in example 1. From fig. 2, it can be seen that the composite material sample is not completely dense based on the CVI method, and the surface layer is more dense than the inner layer; the silicon carbide ceramic matrix composite material reinforced by the 3 layers of carbon nanotube sponges has better density. In addition, the CNTs/SiC ceramic matrix composite reinforced by 3 layers of carbon nano tube sponge can be obtained through measurement, the CNTs are uniformly wrapped by a SiC interface, and the thickness is about 2 mu m; the CNTs are uniformly wrapped by a SiC interface and the thickness of the CNTs/SiC ceramic matrix composite is about 1 mu m;
FIG. 3 is an EDS chart of the composite material prepared in example 1, from which it can be seen that the CNTs/SiC ceramic matrix composite material has a Si content of 85.87 wt.%, a C content of 29.92 wt.%, an O content of 4.62 wt.%, a Na content of 0.56 wt.%, and a Ca content of 0.34 wt.%. Therefore, the composite material prepared by the CVI method has high purity;
FIG. 4 is a 3D confocal microscope image of the composite material prepared in example 1, from which the skeleton and pore structure of the section of the CNTs/SiC ceramic matrix composite material can be more clearly and visually observed.
Table 1 shows the physical property test data of the composite materials prepared in examples 1-3:
Claims (10)
1. carbon nanotube sponge reinforced silicon carbide ceramic matrix compositeThe preparation method of the material is characterized in that carbon nanotube sponge is selected as a prefabricated body, Ar is selected as a carrier gas, and a diluent gas H is used2And introducing trichloromethyl silane MTS into a reaction furnace, heating to 800-1000 ℃, and starting to deposit SiC to obtain the carbon nanotube sponge reinforced silicon carbide ceramic matrix composite.
2. The method of claim 1, wherein the diluent gas H is2The flow rate of (1) is 1500-2000 sccm; the MTS of the trichloromethyl silicon is 150-200 sccm; the flow rate of the argon is 4500-6000 sccm.
3. The production method according to claim 1 or 2, characterized in that the diluent gas H2And trichloromethyl silicone MTS in a volume ratio of (10-11): 1.
4. the production method according to any one of claims 1 to 3, wherein the pressure in the reaction furnace is 9 to 12 KPa.
5. The production method according to any one of claims 1 to 4, wherein the deposition time is 200 to 600 hours.
6. The method according to any one of claims 1 to 5, wherein the temperature is raised at a rate of 3 to 7 ℃/min.
7. The method of any one of claims 1-6, wherein the carbon nanotube sponge is prepared by a method comprising:
mixing a catalyst, an accelerant and a liquid carbon source to obtain a precursor solution;
introducing a mixed gas of argon and hydrogen into a reaction furnace, heating to 1000-1300 ℃, and injecting a precursor solution into the reaction furnace to start the growth of the carbon nano tube;
the obtained carbon nano tube is deposited on a scroll along with carrier gas flow to obtain carbon nano tube sponge;
the catalyst is at least one of ferrocene, cobaltocene and nickelocene; the accelerant is thiophene; the liquid carbon source is at least one of absolute ethyl alcohol, methanol and diethyl ether.
8. The method according to claim 7, wherein the concentration of the catalyst in the precursor solution is 1 to 3 wt%, and the concentration of the accelerator is 0.5 to 1 wt%.
9. The preparation method according to claim 7 or 8, wherein the injection rate of the precursor solution is 18-22 mL/h; the rotating speed of the reel is 4-6 m/min.
10. A carbon nanotube sponge-reinforced silicon carbide ceramic matrix composite prepared according to the preparation method of any one of claims 1 to 9.
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| DAOYANG HAN: "A direct chemical vapor infiltration route for a carbon nanotube/silicon carbide thermal protection system", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| 宋健波: "碳纳米管增强陶瓷基复合材料的研究现状", 《耐火材料》 * |
| 张爱霞等: "一维碳化硅纳米材料的研究进展", 《材料导报》 * |
| 陈兆晨等: "碳化硅颗粒填充的碳纳米管/环氧树脂复合材料的吸波性能", 《功能材料与器件学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116675550A (en) * | 2023-05-29 | 2023-09-01 | 上海大学 | Electromagnetic shielding composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111377750B (en) | 2022-06-24 |
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