CN111392730A - Method for preparing silicon carbide whisker by combining fluidized bed with carbothermic reduction reaction and application thereof - Google Patents
Method for preparing silicon carbide whisker by combining fluidized bed with carbothermic reduction reaction and application thereof Download PDFInfo
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- CN111392730A CN111392730A CN202010322360.9A CN202010322360A CN111392730A CN 111392730 A CN111392730 A CN 111392730A CN 202010322360 A CN202010322360 A CN 202010322360A CN 111392730 A CN111392730 A CN 111392730A
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Abstract
The invention relates to the technical field of silicon carbide whisker preparation, in particular to a method for preparing silicon carbide whiskers by combining a fluidized bed with a carbothermic reduction reaction, which comprises the following steps: (1) heating a fluidized bed reactor, introducing fluidizing gas, and adding a silicon source material from the top of the fluidized bed for fluidizing; (2) introducing carbon source gas from the bottom of the fluidized bed after the silicon source material is stably fluidized; continuously reacting the carbon source gas or the cracking product of the carbon source gas with the silicon source material or the reaction product of the silicon source material to form a silicon carbide crystal nucleus; (3) and the silicon carbide crystal nuclei are transported upwards under the action of the fluidizing gas and attached to the middle upper area of the fluidized bed reactor to grow and form the silicon carbide whiskers. The method has the advantages of simple process flow, convenient operation and realization of large-scale production of the fluidized bed reactor. The production process of the whisker provided by the invention does not need a catalyst, and the product forming region is separated from the silicon source fluidizing region, so that the residue of silicon source powder in the product is effectively avoided, and the purity of the product can be greatly improved.
Description
Technical Field
The invention relates to the technical field of silicon carbide whisker preparation, in particular to a fluidized bed combined carbothermic reduction reaction preparation method of silicon carbide whiskers.
Background
The silicon carbide whisker has high specific strength and specific elastic modulus, has the characteristics of high melting point, corrosion resistance, oxidation resistance and the like, and can be used as a reinforcing and toughening phase for metal matrix, ceramic matrix and polymer matrix composite materials. The current preparation methods of the silicon carbide crystal whisker mainly comprise a carbothermic method, a sol-gel method and a chemical vapor deposition method.
The carbothermic process is a mainstream method for preparing silicon carbide whiskers at present, in which a solid silicon source, a carbon source and a certain catalyst are mixed and reacted at a high temperature to form silicon carbide whiskers. However, carbothermic processes also have a number of problems, including: (1) impurities such as residual carbon source, silicon source, catalyst elements and the like exist in the reaction product, and a complicated separation and purification process flow is required subsequently; (2) the obtained product contains a large amount of silicon carbide powder particles, and the yield of the crystal whiskers is not high; (3) because the reaction space is limited, a large number of bent whiskers exist in the product, the surface of the product is not smooth, and a growth step exists, so that the performance of the reinforcing and toughening effects of the product is limited.
The vapor deposition is cracked by a certain precursor to form the silicon carbide whisker, the quality of the whisker is high, but the preparation process has great defects, which are mainly shown in the following steps: (1) the gas phase reaction is difficult to control effectively, and the integral uniformity of the product is poor; (2) the catalyst needs to be introduced at the same time, and the introduction mode of the catalyst is complex; (3) the concentration of the precursor is low, and the mass production and preparation are difficult.
Disclosure of Invention
The invention aims to provide a method for preparing silicon carbide whiskers by combining a fluidized bed with a carbothermic reduction reaction, which can be used for industrially producing and preparing high-purity silicon carbide whiskers. The production process of the whisker provided by the invention does not need a catalyst, and the product forming region is separated from the silicon source fluidizing region, so that the residue of silicon source powder in the product is effectively avoided, and the purity of the product can be greatly improved.
The first purpose of the invention is realized by the following technical scheme, and the method for preparing the silicon carbide whisker by combining the fluidized bed with the carbothermic reduction reaction comprises the following steps:
(1) heating the fluidized bed reactor to 1000-1700 ℃, introducing fluidizing gas, and adding a silicon source material from the top of the fluidized bed for fluidization;
(2) introducing carbon source gas from the bottom of the fluidized bed after the silicon source material is stably fluidized; continuously reacting the carbon source gas or the cracking product of the carbon source gas with the silicon source material or the reaction product of the silicon source material to form a silicon carbide crystal nucleus;
(3) and the silicon carbide crystal nuclei are transported upwards under the action of the fluidizing gas, separated from the fluidizing zone and attached to the middle upper area of the fluidized bed reactor, and absorb silicon sources and carbon source intermediate products continuously generated at the bottom of the fluidized bed to grow and form silicon carbide whiskers.
Preferably, the silicon source is silicon dioxide, silicon or a mixture of the two.
Preferably, when the silicon source is a mixture of silicon dioxide and silicon, the molar ratio of silicon dioxide to silicon is 10: 1-1: 1.
Preferably, the silicon source is powder or porous microspheres, the particle size is less than 100 microns, and the diameter of the microspheres is 0.1-50 mm.
Preferably, the carbon source gas is any one or any two or more of carbon monoxide, methane, acetylene and propylene.
Preferably, the heating temperature of the silicon source powder is preferably 1200-1500 ℃.
Preferably, the fluidizing gas is argon, hydrogen or nitrogen, and the flow ratio of the fluidizing gas to the carbon source gas is 100: 1-10: 1.
Preferably, the flow ratio of the fluidizing gas to the carbon source gas is preferably 80:1 to 30: 1.
Preferably, the fluidized bed reactor is a hollow cylindrical tube made of graphite, the diameter of the tube is 4-300 cm, and the height of the tube is 0.6-2.0 m.
Preferably, the reaction time of the steps (2) and (3) is 2-4 h.
The second purpose of the invention is to provide the application of the silicon carbide whisker in composite materials, ceramic matrixes, functional coatings or organic slurry.
Compared with the prior art, the invention has the beneficial effects that:
firstly, the carbothermic reduction reaction is introduced into the fluidized bed, the carbon source and the silicon source intermediate product required by the carbothermic reduction reaction are generated in a vapor deposition mode, and uniform mixing is realized in the fluidized bed.
Secondly, no catalyst is introduced in the generation of the intermediate product, and meanwhile, the transport characteristic of the fluidized bed can separate the generation region of the intermediate product from the generation region of the whisker, so that the purity of the whisker is effectively ensured.
Thirdly, the growth mechanism of vapor deposition can ensure that the whisker has long and straight characteristics and a smooth surface state. The invention has simple whole process flow and convenient and fast process operation, and the fluidized bed reactor can realize large-scale production.
Drawings
FIG. 1 is a schematic diagram of the method for preparing silicon carbide whiskers by combining a fluidized bed with a carbothermic reduction reaction according to the invention;
in the figure: 1 is silicon source particle, 2 is silicon carbide crystal nucleus, and 3 is silicon carbide crystal whisker
FIG. 2 is an XRD spectrum of the silicon carbide whisker obtained in example 1 of the present invention;
FIG. 3 is a scanning electron micrograph of the silicon carbide whisker obtained in example 1 of the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
A method for preparing silicon carbide whiskers by combining carbothermic reduction and vapor deposition by utilizing a fluidized bed specifically comprises the following steps:
1) heating the fluidized bed reactor to a certain temperature, introducing fluidizing gas, and adding a silicon source material from the top of the fluidized bed;
2) introducing carbon source gas from the bottom of the fluidized bed after the silicon source material is stably fluidized;
3) continuously reacting the carbon source gas or the cracking product of the carbon source gas with the silicon source material or the reaction product of the silicon source material to form a silicon carbide crystal nucleus;
4) the crystal nucleus is transported upwards under the action of fluidizing gas, separated from the fluidizing zone, attached to the middle upper area of the reactor and grown to form silicon carbide crystal whisker.
The invention combines the carbothermic reduction process with the vapor deposition process, and utilizes the transport characteristic of a fluidized bed to form the silicon carbide whisker, and the basic technical principle is shown in figure 1. The silicon source particles are circularly fluidized in the bottom of the fluidized bed, and the carbon source gas may be introduced while the carbon source gas is introducedAnd interacting with a silicon source to form SiC crystal nuclei. For example, SiO can be reduced by introducing CO2SiO steam is formed, and SiO and CO form SiC crystal nucleuses; hydrocarbon gas is introduced to crack to form nano carbon particles, and the nano carbon particles can also reduce a silicon source to form SiC crystal nuclei; simultaneous addition of Si and SiO2The direct formation of SiO in the fluidized zone can be realized, and the reaction with a carbon source is promoted. The SiC crystal nucleus is transported to the top of the fluidized bed continuously under the action of the fluidizing gas because of extremely small volume, and is attached to the inner wall of the graphite reactor of the fluidized bed when being transported to the middle upper part, and at the moment, intermediate products such as SiO, CO, nano carbon and some hydrocarbons generated in a fluidization area at the bottom are also transported to the area at the same time, and the crystal nucleus grows further to form the crystal whisker.
Example 1
Silicon dioxide is used as a silicon source, the silicon dioxide is added into a fluidized bed in the form of powder, the average diameter of the powder is 100nm, the adding amount of the powder is 50g, the inner diameter of a graphite reactor of the fluidized bed is 6cm, the height of the graphite reactor is 0.8m, a gas distribution plate is arranged at the bottom of the fluidized bed, argon is used as fluidizing gas, the flow rate of the fluidizing gas is 15L/min, the silicon dioxide powder is placed into the fluidized bed for fluidization at 1400 ℃, CO gas and propylene gas are introduced at the moment, the flow rate of CO is 0.5L/min, the flow rate of propylene is 0.3L/min, and the reaction time is 2 h.
The XRD pattern of the reaction product is shown in FIG. 2, and XRD shows that the product is cubic phase silicon carbide and has no other impurity phase. The scanning electron microscope photo (figure 3) of the silicon carbide whisker shows that the diameter of the whisker is 0.2-1.0 micron, the length of the whisker is 5-10 microns, the surface of the whisker is smooth and complete, and no obvious silicon carbide particles are found.
Example 2
The method comprises the steps of adopting a silicon dioxide and silicon mixture as a silicon source, wherein the molar ratio of the silicon dioxide to the silicon is 3:1, adding the silicon source into a fluidized bed in the form of powder, wherein the average diameter of the powder is 5 micrometers, the adding amount is 200g, the inner diameter of a graphite reactor of the fluidized bed is 6cm, the height is 0.8m, arranging a gas distribution plate at the bottom of the fluidized bed, adopting nitrogen as fluidizing gas, the flow rate of the fluidizing gas is 30L/min, placing the silicon source powder into the fluidized bed for fluidization at 1350 ℃, introducing propylene gas at the moment, the flow rate of the propylene is 1. 1.0L/min, and the reaction time is 4 hours.
Example 3
The method comprises the steps of adopting a silicon dioxide and silicon mixture as a silicon source, enabling the molar ratio of the silicon dioxide to the silicon to be 1:1, adding the silicon source into a fluidized bed in the form of spherical particles, enabling the spherical particles to be obtained by two kinds of powder in a rolling forming method, enabling the diameter of the spherical particles to be 800 micrometers, enabling the particles to be subjected to presintering treatment at 1000 ℃ in an inert atmosphere, enabling the adding amount of the spherical particles to be 1000g, enabling the inner diameter of a graphite reactor of the fluidized bed to be 12cm, the height of the graphite reactor to be 1.0m, enabling argon to serve as fluidizing gas, enabling the flow rate of the fluidizing gas to be 50L/min, enabling the silicon source to be placed into the fluidized bed at 1300 ℃ for fluidizing, introducing CO gas and methane gas at the moment, enabling the flow rate.
Example 4
Silicon dioxide is used as a silicon source, the silicon source is added into a fluidized bed in the form of spherical particles, the spherical particles are obtained by a roll forming method, the diameter is 1000 microns, the particles are subjected to presintering treatment in an inert atmosphere at 1000 ℃, the addition amount of the spherical particles is 3000g, the inner diameter of a graphite reactor of the fluidized bed is 250cm, the height of the graphite reactor is 1.6m, argon is used as fluidizing gas, the flow rate of the fluidizing gas is 250L/min, the silicon source is placed into the fluidized bed for fluidization at 1450 ℃, CO gas and acetylene gas are introduced at the moment, the flow rate of CO is 8.0L/min, the flow rate of the acetylene is 6.0L/min, and the reaction time is 2 hours.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (10)
1. A method for preparing silicon carbide whiskers by combining a fluidized bed with a carbothermic reduction reaction is characterized by comprising the following steps:
(1) heating the fluidized bed reactor to 1000-1700 ℃, introducing fluidizing gas, and adding a silicon source material from the top of the fluidized bed for fluidization;
(2) introducing carbon source gas from the bottom of the fluidized bed after the silicon source material is stably fluidized; continuously reacting the carbon source gas or the cracking product of the carbon source gas with the silicon source material or the reaction product of the silicon source material to form a silicon carbide crystal nucleus;
(3) and the silicon carbide crystal nuclei are transported upwards under the action of the fluidizing gas, separated from the fluidizing zone and attached to the middle upper area of the fluidized bed reactor, and absorb silicon sources and carbon source intermediate products continuously generated at the bottom of the fluidized bed to grow and form silicon carbide whiskers.
2. The method for preparing silicon carbide whiskers by using a fluidized bed combined with a carbothermic reduction reaction according to claim 1, wherein the silicon source is silicon dioxide, silicon or a mixture of silicon dioxide and silicon.
3. The method for preparing the silicon carbide whiskers by utilizing the combination of the fluidized bed and the carbothermic reduction reaction according to any one of claims 1 or 2, wherein the silicon source is powder or porous microspheres, and the diameter of the microspheres is 0.1-50 mm.
4. The method for preparing the silicon carbide whiskers by utilizing the combination of the fluidized bed and the carbothermic reduction reaction according to claim 1 or 2, wherein the carbon source gas is any one or two or more of carbon monoxide, methane, acetylene and propylene.
5. The method for preparing the silicon carbide whiskers by utilizing the combination of the fluidized bed and the carbothermic reduction reaction as described in claim 1 or 2, wherein the fluidizing gas is argon, hydrogen or nitrogen, and the flow ratio of the fluidizing gas to the carbon source gas is 100: 1-10: 1.
6. The method for preparing silicon carbide whiskers by utilizing a fluidized bed in combination with a carbothermic reduction reaction according to claim 1 or 2, wherein the fluidized bed reactor is a hollow cylindrical tube made of graphite, the diameter of the tube is 4-300 cm, and the height of the tube is 0.6-2.0 m.
7. The method for preparing silicon carbide whiskers by using a fluidized bed combined with a carbothermic reduction reaction according to claim 1 or 2, wherein the reaction time of step (2) and step (3) is 2-4 h.
8. The method for preparing the silicon carbide whiskers by using the combination of the fluidized bed and the carbothermic reduction reaction according to claim 1 or 2, wherein the fluidized bed reactor is heated to 1200-1500 ℃.
9. The method for preparing the silicon carbide whiskers by utilizing the combination of the fluidized bed and the carbothermic reduction reaction as described in claim 4, wherein the flow ratio of the fluidizing gas to the carbon source gas is 80: 1-30: 1.
10. Use of the silicon carbide whiskers obtained by the method of any one of claims 1-9 in a composite material, a ceramic substrate, a functional coating or an organic slurry.
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Cited By (5)
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| CN112133915A (en) * | 2020-08-13 | 2020-12-25 | 利普同呈(江苏)新能源科技有限公司 | Preparation method of silicon-carbon composite material |
| CN112923733A (en) * | 2021-02-02 | 2021-06-08 | 北京绿清科技有限公司 | Method for producing silicon carbide by adopting multi-furnace series connection grading melting furnace and special production system |
| CN112978732A (en) * | 2021-02-02 | 2021-06-18 | 北京绿清科技有限公司 | Production method and special production system of silicon carbide |
| CN114751759A (en) * | 2021-07-06 | 2022-07-15 | 浙江天鹰机械密封件股份有限公司 | Preparation method of friction pair material of mechanical sealing element |
| CN115939402A (en) * | 2023-01-09 | 2023-04-07 | 天目湖先进储能技术研究院有限公司 | Silicon-based material, preparation method thereof and application thereof in negative electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115939402A (en) * | 2023-01-09 | 2023-04-07 | 天目湖先进储能技术研究院有限公司 | Silicon-based material, preparation method thereof and application thereof in negative electrode |
| CN115939402B (en) * | 2023-01-09 | 2023-05-30 | 天目湖先进储能技术研究院有限公司 | Silicon-based material, preparation method thereof and application thereof in negative electrode |
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