CN117466645A - Aluminum silicide whisker and preparation method thereof - Google Patents

Aluminum silicide whisker and preparation method thereof Download PDF

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CN117466645A
CN117466645A CN202311811748.5A CN202311811748A CN117466645A CN 117466645 A CN117466645 A CN 117466645A CN 202311811748 A CN202311811748 A CN 202311811748A CN 117466645 A CN117466645 A CN 117466645A
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aluminum
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甄强
李文豪
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Zhejiang Lab
University of Shanghai for Science and Technology
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Zhejiang Lab
University of Shanghai for Science and Technology
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Abstract

The invention belongs to the technical field of ceramic materials, and relates to an aluminum silicide whisker and a preparation method thereof, wherein the preparation method comprises the following steps: mixing a catalyst, a solvent, an aluminum source, a silicon source and a carbon source, drying, burying carbon, and sintering to obtain carbon aluminum silicide whiskers; wherein the catalyst is one or a combination of a plurality of nickel-based catalyst, iron-based catalyst or cobalt-based catalyst. Compared with the prior art, the aluminum silicide carbon whisker prepared by the method has uniform thickness and larger specific surface area; the unique two-dimensional linear structure of the aluminum silicide whisker has better wrapping property on the inside of the ceramic material, can play a role in bridging a bracket, and can be oxidized at first during high-temperature oxidation; by changing the types of the catalysts, the aluminum silicide carbon whiskers with different sizes can be prepared, so that the dimension controllability of the aluminum silicide carbon whiskers is realized, and the production requirements of different industries can be met.

Description

Aluminum silicide whisker and preparation method thereof
Technical Field
The invention belongs to the technical field of ceramic materials, and relates to an aluminum carbide whisker and a preparation method thereof.
Background
Ceramic materials are widely used in various fields of national economy such as national defense, chemical industry, metallurgy, electronics, machinery, aviation, aerospace, biomedicine and the like due to a series of excellent performances such as high strength, high hardness, wear resistance, corrosion resistance, high temperature resistance, conductivity, insulation, magnetism, light transmittance, semiconductors, piezoelectricity, ferroelectricity, acousto-optic, superconductivity, biocompatibility and the like. However, the ceramic material has the fatal disadvantages of large brittleness, low impact resistance and brittleness. At present, ceramic whiskers are introduced into a ceramic matrix to remarkably improve the fracture toughness of a ceramic material, and the toughness and strength of the ceramic are improved through mechanisms such as crack deflection bending, debonding effect, pulling effect, whisker bridging and the like.
The ceramic whiskers commonly used at present mainly comprise: oxide whiskers (e.g. Al 2 O 3 MgO, znO, mullite), carbide whiskers (e.g., siC, tiC, nbC), and nitride whiskers (e.g., si) 3 N 4 AlN), and the like. Chinese patents CN113666749a and CN108928821a report ternary carbide aluminum carbosilicide (i.e., al 4 SiC 4 ) The ceramic has a low density (3.03 g/cm 3 ) Higher melting point (> 2700 ℃), low thermal expansion coefficient and excellent oxidation and hydration resistance. But for Al 4 SiC 4 Whisker growth studies on ceramics have not been reported.
Therefore, how to directionally grow the aluminum carbide ceramic into whiskers so as to further improve the toughness of the aluminum carbide ceramic becomes a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide an aluminum silicide whisker and a preparation method thereof, which are used for solving the problem of poor toughness of aluminum silicide ceramics.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of carbon aluminum silicide whisker comprises the following steps:
mixing a catalyst, a solvent, an aluminum source, a silicon source and a carbon source, drying, burying carbon, and sintering to obtain carbon aluminum silicide whiskers; wherein the catalyst is one or a combination of a plurality of nickel-based catalyst, iron-based catalyst or cobalt-based catalyst.
Further, the nickel-based catalyst is nickel nitrate or nickel acetylacetonate; the iron-based catalyst is ferric nitrate or ferric acetylacetonate; the cobalt-based catalyst is cobalt nitrate or cobalt acetylacetonate.
Further, the solvent is selected from one or more of alcohol solvents, ketone solvents or ester solvents.
Further, the aluminum source is aluminum powder, the silicon source is silicon powder, and the carbon source is graphite powder.
Further, the particle size of the catalyst is more than or equal to 50 mu m; the grain diameter of the aluminum powder is less than or equal to 100 mu m; the particle size of the graphite powder is less than or equal to 50 mu m; the grain diameter of the silicon powder is less than or equal to 100 mu m.
Further, the mixing process of the catalyst, the solvent, the aluminum source, the silicon source and the carbon source comprises the following steps: firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, and then adding an aluminum source, a silicon source and a carbon source for ball milling and mixing.
Further, in the mixture composed of the catalyst, an aluminum source, a silicon source and a carbon source, the mass contents of the components are as follows: 22-28% of aluminum source, 41-47% of silicon source, 27-33% of carbon source and 0.7-1.3% of catalyst.
Further, in the drying process, the drying temperature is 80-120 ℃, and the drying time is 5-10 hours.
Further, in the carbon embedding sintering process, the sintering temperature is 1400-1500 ℃ and the sintering time is 1-4 hours.
The carbon aluminum silicide whisker is prepared by the method.
Compared with the prior art, the invention has the following characteristics:
1) The invention adopts a simple one-pot method for mixing, takes aluminum powder, silicon powder and graphite powder as the preparation raw materials of the aluminum silicide whiskers, and the aluminum silicide whiskers are catalytically grown by a gas-liquid-solid mechanism under the action of a catalyst, and the obtained aluminum silicide (Al 4 SiC 4 ) The whisker has uniform thickness and larger specific surface area; the unique two-dimensional linear structure of the aluminum silicide whisker has better wrapping property on the inside of the ceramic material, can play a role in bridging a bracket, and can be oxidized at first during high-temperature oxidation; by changing the types of the catalysts, the aluminum silicide whiskers with different sizes can be prepared, thereby realizing the controllability of the sizes of the aluminum silicide whiskers and meeting the production requirements of different industries. The results of the examples show that the average diameter of the aluminum silicide carbide whisker prepared by the preparation method provided by the invention is 50-1000 nm;
2) The invention has the advantages of wide sources of raw materials, low cost, simple preparation method, good repeatability and short production period, and is suitable for industrial production.
Drawings
FIG. 1 is an SEM image of an aluminum silicide carbide whisker prepared in example 1 of the invention;
FIG. 2 is a line scan (EDS) diagram of an aluminum silicide carbide whisker prepared in example 1 of the present invention;
FIG. 3 is an XRD pattern of aluminum silicide carbide whiskers prepared in example 1 of the invention;
FIG. 4 is an SEM image of an aluminum silicide carbide whisker prepared in example 2 of the invention;
FIG. 5 is an SEM image of an aluminum silicide carbide whisker prepared in example 3 of the invention;
fig. 6 is an SEM image of aluminum carbosilicide prepared in comparative example 1.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
The invention provides a preparation method of carbon aluminum silicide whisker, which comprises the following steps:
(1) Mixing a catalyst, a solvent, aluminum powder, silicon powder and graphite powder to obtain a mixture; wherein the catalyst comprises one or more of a nickel-based catalyst, an iron-based catalyst and a cobalt-based catalyst;
(2) And (3) sequentially carrying out drying treatment and carbon embedding sintering on the mixture obtained in the step (1) to obtain the carbon aluminum silicide whisker.
The invention mixes the catalyst, solvent, aluminum powder, silicon powder and graphite powder to obtain a mixture. The specific sources of the catalyst, the solvent, the aluminum powder, the silicon powder and the graphite powder are not particularly limited, and commercially available products well known to those skilled in the art can be adopted.
In the present invention, the mixture of the catalyst, the solvent, the aluminum powder, the silicon powder and the graphite powder is particularly preferably: firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, and then adding aluminum powder, silicon powder and graphite powder for ball milling and mixing. By adopting the mode for mixing, the invention can ensure that the components are mixed more uniformly.
In the invention, the ultrasonic dissolution time is preferably 30-60 min, more preferably 40-60 min, and even more preferably 50-55 min. The power of the ultrasonic dissolution is not particularly limited, and may be determined according to the technical common knowledge of a person skilled in the art. The invention can fully disperse the catalyst in the solvent through ultrasonic dissolution.
In the present invention, the ball-milling mixing is preferably performed in a ball-milling tank; the ball milling and mixing time is preferably 2-3 hours, more preferably 2.5-3 hours, and even more preferably 2.5 hours. The rotational speed of the ball mill during mixing is not particularly limited, and the rotational speed is determined according to the technical common knowledge of a person skilled in the art. The invention can fully and uniformly mix the components by ball milling and mixing.
In the present invention, the catalyst preferably includes one or more of a nickel-based catalyst, an iron-based catalyst, and a cobalt-based catalyst. In the present invention, the nickel-based catalyst is preferably nickel nitrate or nickel acetylacetonate; the iron-based catalyst is preferably ferric nitrate or ferric acetylacetonate; the cobalt-based catalyst is preferably cobalt nitrate or cobalt acetylacetonate. According to the invention, different catalysts are adopted, so that the aluminum silicide carbon whiskers with different sizes can be prepared, and the production requirements of different industries are met.
In the invention, the particle size of the catalyst is preferably not less than 50 μm, more preferably 50-100 μm, and even more preferably 60-80 μm; the purity of the catalyst is preferably not less than 98%, more preferably not less than 99%, and further preferably not less than 99%. In the invention, the particle size of the aluminum powder is preferably not more than 100 μm, more preferably 50 to 100 μm, and even more preferably 60 to 70 μm; the purity of the aluminum powder is preferably not less than 98%, more preferably 98 to 99%, and even more preferably 99%. In the invention, the particle size of the graphite powder is preferably not more than 50 μm, more preferably 35 to 50 μm, and even more preferably 40 to 50 μm; the purity of the graphite powder is preferably more than or equal to 98%, more preferably 98-98.5%. In the invention, the grain diameter of the silicon powder is preferably less than or equal to 100 mu m, more preferably 50-100 mu m, and even more preferably 60-80 mu m; the purity of the silicon powder is preferably more than or equal to 2N, and more preferably 2N-3N. According to the invention, by controlling the granularity and purity of the raw materials, on one hand, the raw materials can be mixed more fully and are easier to generate chemical reaction, and on the other hand, the content of impurities can be reduced.
In the present invention, the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is preferably 100 percent: 22-28% of aluminum powder, 41-47% of silicon powder, 27-33% of graphite powder and 0.7-1.3% of catalyst, and more preferably: 23-27% of aluminum powder, 42-46% of silicon powder, 28-32% of graphite powder and 0.8-1.2% of catalyst, and more preferably: 24-26% of aluminum powder, 43-45% of silicon powder, 29-31% of graphite powder and 0.9-1.1% of a catalyst. The invention can make most raw materials generate carbon aluminum silicide whisker under the action of catalyst by controlling the dosage of each component, the carbon aluminum silicide whisker is catalyzed and grown by a gas-liquid-solid mechanism, and the obtained carbon aluminum silicide whisker has uniform thickness and larger specific surface area.
In the present invention, the solvent preferably includes one or more of an alcohol solvent, a ketone solvent and an ester solvent, more preferably one or more of ethanol, acetone and ethyl acetate, and still more preferably ethanol. The invention can further uniformly mix the raw materials by adopting the solvent.
The invention has no special limit to the dosage of the solvent, and can ensure that the components are fully dissolved or uniformly mixed.
After the mixture is obtained, the invention sequentially carries out drying treatment and carbon embedding sintering on the mixture to obtain the carbon aluminum silicide whisker.
In the invention, the temperature of the drying treatment is preferably 80-120 ℃, more preferably 90-110 ℃, and even more preferably 100 ℃; the drying time is preferably 5 to 10 hours, more preferably 6 to 9 hours, and even more preferably 7 to 8 hours. According to the invention, through drying treatment, the solvent in the mixture can be removed, so that the subsequent carbon-embedded sintering is facilitated.
In the invention, the temperature of the carbon-embedded sintering is preferably 1400-1500 ℃, more preferably 1425-1475 ℃, and even more preferably 1450 ℃; the time for carbon embedding and sintering is preferably 1 to 4 hours, more preferably 2 to 3 hours, and even more preferably 2.5 hours. According to the invention, through controlling parameters of carbon implantation sintering, during the sintering process, under the action of a catalyst, the carbon aluminum silicide whisker grows in a large quantity by a V-L-S (gas-liquid-solid) growth mechanism.
According to the invention, a simple one-pot method is adopted for mixing, aluminum powder, silicon powder and graphite powder are used as preparation raw materials of the aluminum silicide whiskers, the aluminum silicide whiskers are catalytically grown by a gas-liquid-solid mechanism under the action of a catalyst, and the obtained aluminum silicide whiskers are uniform in thickness and have larger specific surface area; the unique two-dimensional linear structure of the aluminum silicide whisker has better wrapping property on the inside of the ceramic material, can play a role in bridging a bracket, and can be oxidized at first during high-temperature oxidation; by changing the types of the catalysts, the aluminum silicide carbon whiskers with different sizes can be prepared, and the production requirements of different industries can be met; the adopted raw materials have wide sources and low price, the preparation method is simple, the repeatability is good, the production period is short, and the method is suitable for industrial production.
The invention provides the aluminum silicide carbide whisker prepared by the preparation method. In the invention, the average diameter of the aluminum silicide carbide whiskers is preferably 50-1000 nm.
The invention provides application of the carbon aluminum silicide whisker in the fields of national defense, chemical industry, metallurgy, electronics, machinery, aviation, aerospace and biomedicine. The specific mode of the application of the present invention is not particularly limited, and modes well known to those skilled in the art can be adopted.
The following examples are given with the above technical solutions of the present invention as a premise, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples.
Example 1: nickel nitrate as catalyst
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution for 55min, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing for 2.5h in a ball milling tank to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
FIG. 1 is an SEM image of an aluminum silicide carbide whisker prepared in example 1 of the invention. As can be seen from FIG. 1, the average diameter of the synthesized aluminum silicide carbide whiskers is 1 μm (1000 nm).
FIG. 2 is a line scan (EDS) diagram of an aluminum silicide carbide whisker prepared in example 1 of the present invention. As can be seen from fig. 2, the aluminum silicide whiskers are mainly composed of aluminum, silicon and carbon, and nickel is gathered on the top of the whiskers, so that the growth of the aluminum silicide whiskers accords with a gas-liquid-solid growth mechanism.
TABLE 1 EDS line scan element content
Element name Element symbol Atomic percent (%) Weight percent (wt%)
Aluminum (Al) Al 50.22 67.79
Carbon (C) C 47.36 28.45
Silicon (Si) Si 2.19 3.08
Nickel (Ni) Ni 0.23 0.68
Figure 3 is an XRD pattern of an aluminum silicide carbide whisker prepared in example 1 of the present invention. As can be seen from fig. 3, the XRD pattern is mainly composed of diffraction peaks of aluminum silicide carbide, siC and graphite C, because excessive Si powder and graphite C powder are added into the reaction system, and part of Si powder and graphite C powder react to generate SiC in the high-temperature sintering process. As can be seen from fig. 2 to 3, the aluminum silicide whiskers are catalytically grown under the action of the catalyst.
Example 2: iron nitrate as catalyst
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution for 55min, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing for 2.5h in a ball milling tank to obtain a mixture;
wherein the catalyst is ferric nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
Fig. 4 is an SEM image of aluminum silicide carbide whiskers prepared in example 2 of the present invention. As can be seen from FIG. 4, the average diameter of the synthesized aluminum silicide whiskers is 200nm.
Example 3: cobalt nitrate as catalyst
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution for 55min, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing for 2.5h in a ball milling tank to obtain a mixture;
the catalyst is cobalt nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
Fig. 5 is an SEM image of aluminum silicide carbide whiskers prepared in example 3 of the present invention. As can be seen from FIG. 5, the average diameter of the synthesized aluminum silicide whiskers is 80nm.
Comparative example 1: no catalyst
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Adding aluminum powder, silicon powder and graphite powder into a solvent, and ball-milling and mixing the mixture in a ball-milling tank for 2.5 hours to obtain a mixture;
wherein the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 45% of silicon powder and 30% of graphite powder;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
Fig. 6 is an SEM image of aluminum carbosilicide prepared in comparative example 1. As can be seen from fig. 6, the synthesized aluminum silicide contains no whiskers.
As can be seen from comparison of examples 1 to 3 and comparative example 1, by adding the catalyst when preparing aluminum silicide, the growth of aluminum silicide whiskers can be promoted, while when not adding the catalyst, aluminum silicide whiskers are not generated, and meanwhile, different types of catalysts are adopted, so that the sizes of the obtained aluminum silicide whiskers are different, which indicates that the controllability of the aluminum silicide whiskers can be realized by controlling the types of the catalysts.
Example 4: different ultrasound times
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing in a ball milling tank for 2.5 hours to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst; the ultrasonic dissolution time is respectively 30min, 40min, 50min, 52min, 55min and 60min;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
Example 5: different ball milling time
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing in a ball milling tank to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst; the ball milling time is respectively 2h, 2.5h and 3h;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
Example 6: different mass contents of aluminum powder, silicon powder, graphite powder and catalyst
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution for 55min, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing for 2.5h in a ball milling tank to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvents are ethanol, acetone and ethyl acetate respectively; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent respectively:
22% of aluminum powder, 43.7% of silicon powder, 33% of graphite powder and 1.3% of catalyst;
28% of aluminum powder, 44.3% of silicon powder, 27% of graphite powder and 0.7% of catalyst;
27% of aluminum powder, 41% of silicon powder, 31.2% of graphite powder and 0.8% of catalyst;
23% of aluminum powder, 47% of silicon powder, 28.8% of graphite powder and 1.2% of catalyst;
24% of aluminum powder, 46% of silicon powder, 28.9% of graphite powder and 1.1% of catalyst;
26% of aluminum powder, 42% of silicon powder, 31% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
Example 7: different solvents
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution for 55min, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing for 2.5h in a ball milling tank to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvents are ethanol, acetone and ethyl acetate respectively; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5h.
Example 8: different drying temperatures
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing in a ball milling tank for 2.5 hours to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 80 ℃, 90 ℃, 100 ℃, 110 ℃, 120 ℃ and the time of the drying treatment is 7 hours; the temperature of carbon embedding and sintering is 1450 ℃ respectively, and the time of carbon embedding and sintering is 2.5h.
Example 9: different drying times
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing in a ball milling tank for 2.5 hours to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 5 hours, 6 hours, 7 hours, 8 hours, 9 hours and 10 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 2.5 hours respectively.
Example 10: different carbon-embedding sintering temperatures
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing in a ball milling tank for 2.5 hours to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the temperature of the carbon embedding sintering is 1400 ℃, 1425 ℃, 1450 ℃, 1475 ℃ and 1500 ℃ respectively, and the time of the carbon embedding sintering is 2.5 hours.
Example 11: different carbon-embedding sintering time
The preparation method of the carbon aluminum silicide whisker comprises the following steps:
(1) Firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, then adding aluminum powder, silicon powder and graphite powder, and performing ball milling and mixing in a ball milling tank for 2.5 hours to obtain a mixture;
the catalyst is nickel nitrate, the particle size of the catalyst is 60-80 mu m, and the purity of the catalyst is more than or equal to 98%; the grain diameter of the aluminum powder is 60-70 mu m, and the purity of the aluminum powder is more than or equal to 98%; the particle size of the graphite powder is 40-50 mu m, and the purity of the graphite powder is more than or equal to 98%; the grain diameter of the silicon powder is 60-80 mu m, and the purity of the silicon powder is more than or equal to 2N; the solvent is ethanol; the total mass of the aluminum powder, the silicon powder, the graphite powder and the catalyst is 100 percent: 25% of aluminum powder, 44% of silicon powder, 30% of graphite powder and 1% of catalyst;
(2) Sequentially drying the mixture obtained in the step (1) and burying carbon for sintering to obtain carbon aluminum silicide whiskers; the temperature of the drying treatment is 100 ℃, and the time of the drying treatment is 7 hours; the carbon embedding sintering temperature is 1450 ℃, and the carbon embedding sintering time is 1h, 2.5h, 3h and 4h respectively.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.

Claims (10)

1. The preparation method of the carbon aluminum silicide whisker is characterized by comprising the following steps:
mixing a catalyst, a solvent, an aluminum source, a silicon source and a carbon source, drying, burying carbon, and sintering to obtain carbon aluminum silicide whiskers; wherein the catalyst is one or a combination of a plurality of nickel-based catalyst, iron-based catalyst or cobalt-based catalyst.
2. The method for preparing aluminum silicide carbon whisker according to claim 1, wherein the nickel-based catalyst is nickel nitrate or nickel acetylacetonate; the iron-based catalyst is ferric nitrate or ferric acetylacetonate; the cobalt-based catalyst is cobalt nitrate or cobalt acetylacetonate.
3. The method for preparing aluminum silicide carbon whisker according to claim 1, wherein the solvent is one or more selected from alcohol solvents, ketone solvents and ester solvents.
4. The method for preparing aluminum silicide carbon whisker according to claim 1, wherein the aluminum source is aluminum powder, the silicon source is silicon powder, and the carbon source is graphite powder.
5. The method for preparing carbon aluminum silicide whisker according to claim 4, wherein the particle size of the catalyst is not less than 50 μm; the grain diameter of the aluminum powder is less than or equal to 100 mu m; the particle size of the graphite powder is less than or equal to 50 mu m; the grain diameter of the silicon powder is less than or equal to 100 mu m.
6. The method for preparing carbon aluminum silicide whisker according to claim 1, wherein the mixing process of the catalyst, the solvent, the aluminum source, the silicon source and the carbon source comprises: firstly, mixing a catalyst and a solvent, then performing ultrasonic dissolution, and then adding an aluminum source, a silicon source and a carbon source for ball milling and mixing.
7. The preparation method of the carbon aluminum silicide whisker according to claim 1, wherein the mixture consisting of the catalyst, an aluminum source, a silicon source and a carbon source comprises the following components in percentage by mass: 22-28% of aluminum source, 41-47% of silicon source, 27-33% of carbon source and 0.7-1.3% of catalyst.
8. The method for preparing the aluminum silicide carbon whisker according to claim 1, wherein in the drying process, the drying temperature is 80-120 ℃ and the drying time is 5-10 h.
9. The method for preparing the carbon aluminum silicide whisker according to claim 1, wherein in the carbon implantation sintering process, the sintering temperature is 1400-1500 ℃ and the sintering time is 1-4 h.
10. An aluminium silicide carbon whisker prepared by the method of any one of claims 1 to 9.
CN202311811748.5A 2023-12-27 2023-12-27 Aluminum silicide whisker and preparation method thereof Pending CN117466645A (en)

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