CN109437913B - Method for preparing silicon carbide ceramic powder by low-temperature synthesis - Google Patents
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Abstract
A method for preparing silicon carbide ceramic powder by low-temperature synthesis comprises the following steps: (1) sequentially adding water glass, a coupling agent, polyethylene glycol and hydrochloric acid into deionized water, and stirring to prepare gel; filtering after water washing and alcohol washing; (2) adding into anhydrous ethanol, adding phenolic resin under stirring, and stirring to form paste; drying at 65-200 ℃, cooling to be ground; (3) putting the mixture into a heating furnace, introducing argon and keeping the mixture flowing; heating to 1400-1550 ℃ for carbothermic reduction reaction, and cooling along with the furnace; (4) and (3) placing the mixture into a resistance furnace, preserving heat at 550-650 ℃ to remove residual carbon, cooling the mixture to normal temperature along with the furnace, and grinding the mixture. The method has wide raw material sources, and the silicon source and the carbon source are uniformly mixed at an atomic or molecular level by means of catalytic modification and the like, so that the temperature of the carbothermic reduction reaction is reduced, and the production cost is reduced.
Description
Technical Field
The invention belongs to the field of inorganic non-metallic materials, and particularly relates to a method for preparing silicon carbide ceramic powder through low-temperature synthesis.
Background
Silicon carbide (SiC) ceramic has excellent performances such as high temperature resistance, corrosion resistance, high hardness, high strength and the like, and is concerned, and with the continuous development of high and new technical fields, silicon carbide ceramic materials have wide development prospects in high-tech fields such as refractory materials, metallurgy, machinery, chemical engineering, military industry and the like; but the main problems existing at present are that the production cost of the silicon carbide ceramic is high, and the commercial popularization and application of the silicon carbide ceramic material are seriously influenced; for this reason, there is an urgent need to reduce the production cost of silicon carbide ceramic materials.
One of the effective ways to reduce the production cost of the silicon carbide ceramic material is to reduce the production cost of the production raw material (silicon carbide ceramic powder); at present, the most commercially popularized production method of silicon carbide ceramic powder is a method combining a wet chemical method and a carbothermic reduction method, and has the main problems that the carbothermic reduction reaction temperature is higher, generally about 1550-1650 ℃, the agglomeration phenomenon is serious, a commonly used silicon source is mainly tetraethoxysilane, and the price is higher; therefore, agglomeration is inhibited, the carbothermic reduction reaction temperature is lowered, and the price of the silicon source is imperative.
Disclosure of Invention
The invention aims to provide a method for preparing silicon carbide ceramic powder by low-temperature synthesis, which prepares high-purity silicon carbide on the basis of low-temperature synthesis by selecting raw materials and matching with a process flow, reduces the cost and improves the production efficiency.
The method of the invention comprises the following steps:
1. preparing a gel: preparing silicon source water glass, catalyst hydrochloric acid, surfactant coupling agent and polyethylene glycol, wherein the mass concentration of the hydrochloric acid is 5-35%; the hydrochloric acid accounts for 1-30% of the volume of the water glass, the coupling agent accounts for 0.01-10.0% of the total volume of the water glass and the hydrochloric acid, and the polyethylene glycol accounts for 0.01-10.0% of the total mass of the water glass and the hydrochloric acid; sequentially adding water glass, a coupling agent, polyethylene glycol and hydrochloric acid into deionized water, and uniformly stirring to prepare gel; washing the gel with water and alcohol, and filtering to obtain precursor gel;
2. preparing precursor powder: putting the precursor gel into absolute ethyl alcohol, adding phenolic resin under the stirring condition, dissolving the phenolic resin in the absolute ethyl alcohol, and dispersing the precursor gel until all materials form a paste; putting the paste body into an oven, drying at 65-200 ℃ to remove volatile components, cooling the residual materials to normal temperature along with the oven, taking out and grinding to prepare precursor powder; wherein the molar ratio of the phenolic resin to the water glass is 0.5-10;
3. synthesizing: putting the precursor powder into a heating furnace, introducing argon into the heating furnace to remove air, and keeping the argon flowing; then heating the heating furnace to 1400-1550 ℃, preserving heat for 2-5 hours, carrying out carbothermic reduction reaction, and cooling to normal temperature along with the furnace after the reaction is finished to obtain coarse powder;
4. decarbonization: and (3) placing the coarse powder into a resistance furnace, preserving heat for 2-8 hours at 550-650 ℃ to remove residual carbon, cooling the reacted materials to normal temperature along with the furnace, and grinding to prepare the silicon carbide ceramic powder.
The polymerization degree of the polyethylene glycol is 2000-20000.
In the step 1, the dosage of the deionized water is based on that the water glass, the coupling agent and the polyethylene glycol are completely dissolved after the deionized water is mixed with the hydrochloric acid.
In the step 2, the amount of the absolute ethyl alcohol is based on the total dissolution of the phenolic resin.
The grain diameter of the silicon carbide ceramic powder is 200-1000 nanometers.
The silicon source adopted by the invention is water glass with low price and wide source, and replaces tetraethoxysilane with higher price, and the carbon source adopts phenolic resin with higher carbon content and low price; because the water glass and the phenolic resin are mutually incompatible and are completely mixed by machinery, the water glass and the phenolic resin are difficult to be uniformly mixed at an atomic or molecular level, the water glass is promoted to be hydrolyzed by the catalytic action of hydrochloric acid, and the colloidal particles are dispersed and surface-modified by combining the grafting, surface modification and dispersing actions of the coupling agent and the polyethylene glycol, even if the silicon source and the carbon source are compatible and are uniformly mixed at the atomic or molecular level, so that the carbothermic reduction reaction temperature is reduced, and the production cost is reduced.
Drawings
FIG. 1 is an X-ray diffraction chart of a silicon carbide ceramic powder in example 1 of the present invention;
FIG. 2 is an SEM photograph of the silicon carbide ceramic powder in example 1 of the present invention.
Detailed Description
The water glass, the coupling agent, the polyethylene glycol and the phenolic resin adopted in the embodiment of the invention are commercial products.
The embodiment of the invention adopts an X-ray diffractometer with the model number of PW 3040/60.
The scanning electron microscope adopted in the embodiment of the invention is SSX-550 in model.
In the embodiment of the invention, the water washing and the alcohol washing are that the gel is firstly put into water and stirred for at least 5min, and then taken out and put into ethanol and stirred for at least 5 min.
In the embodiment of the invention, the drying time is 2-24 hours at 65-200 ℃.
In the embodiment of the invention, the coupling agent is KH-550, KH-560 or KH-570.
In the embodiment of the invention, FQ-9 is selected as the phenolic resin.
Example 1
Preparing silicon source water glass, catalyst hydrochloric acid, surfactant coupling agent and polyethylene glycol, wherein the mass concentration of the hydrochloric acid is 35%; the hydrochloric acid accounts for 1 percent of the volume of the water glass, the coupling agent accounts for 0.01 percent of the total volume of the water glass and the hydrochloric acid, and the polyethylene glycol accounts for 0.01 percent of the total mass of the water glass and the hydrochloric acid; sequentially adding water glass, a coupling agent, polyethylene glycol and hydrochloric acid into deionized water, and uniformly stirring to prepare gel; washing the gel with water and alcohol, and filtering to obtain a solid phase as precursor gel; wherein the polymerization degree of the polyethylene glycol is 2000; the dosage of the deionized water is based on that the deionized water is mixed with hydrochloric acid and then the water glass, the coupling agent and the polyethylene glycol are completely dissolved;
putting the precursor gel into absolute ethyl alcohol, adding phenolic resin under the stirring condition, dissolving the phenolic resin in the absolute ethyl alcohol, and dispersing the precursor gel until all materials form a paste; putting the paste body into an oven, drying at 65 ℃ to remove volatile components, cooling the residual materials to normal temperature along with the oven, taking out and grinding to prepare precursor powder; the dosage of the absolute ethyl alcohol is based on the dissolution of all the phenolic resin; the molar ratio of the phenolic resin to the water glass is 2;
putting the precursor powder into a heating furnace, introducing argon into the heating furnace to remove air, and keeping the argon flowing; then heating the heating furnace to 1400 ℃, preserving the temperature for 5 hours, carrying out carbothermic reduction reaction, and cooling the obtained product to normal temperature along with the furnace after the reaction is finished to obtain coarse powder;
placing the coarse powder in a resistance furnace, preserving heat for 8 hours at 550 ℃ to remove residual carbon, cooling the reacted materials to normal temperature along with the furnace, grinding the materials to prepare silicon carbide ceramic powder with the particle size of 100-350 nanometers, wherein the X-ray diffraction result is shown in figure 1, the product has no obvious impurities, and the SEM photograph of the silicon carbide powder is shown in figure 2.
Example 2
The method is the same as example 1, except that:
(1) the mass concentration of the hydrochloric acid is 25 percent; the hydrochloric acid accounts for 10 percent of the volume of the water glass, the coupling agent accounts for 1 percent of the total volume of the water glass and the hydrochloric acid, and the polyethylene glycol accounts for 1 percent of the total mass of the water glass and the hydrochloric acid; the polymerization degree of the polyethylene glycol is 4000;
(2) the mol ratio of the phenolic resin to the water glass is 5, and the paste is dried at the temperature of 80 ℃ to remove volatile components;
(3) heating the heating furnace to 1450 ℃, and preserving the temperature for 4 hours to carry out carbothermic reduction reaction;
(4) and (3) preserving the heat of the coarse powder for 6 hours at the temperature of 600 ℃ to remove residual carbon, cooling the reacted material to normal temperature along with a furnace, and grinding and crushing the cooled material to prepare silicon carbide ceramic powder with the particle size of 200-450 nanometers.
Example 3
The method is the same as example 1, except that:
(1) the mass concentration of the hydrochloric acid is 15 percent; the hydrochloric acid accounts for 20% of the volume of the water glass, the coupling agent accounts for 5% of the total volume of the water glass and the hydrochloric acid, and the polyethylene glycol accounts for 10% of the total mass of the water glass and the hydrochloric acid; the polymerization degree of the polyethylene glycol is 6000;
(2) the mol ratio of the phenolic resin to the water glass is 8, and the paste is dried at 120 ℃ to remove volatile components;
(3) heating the heating furnace to 1500 ℃, preserving the heat for 3 hours, and carrying out carbothermic reduction reaction;
(4) and (3) preserving the heat of the coarse powder for 4 hours at the temperature of 620 ℃ to remove residual carbon, cooling the reacted material to normal temperature along with a furnace, and grinding and crushing the cooled material to prepare silicon carbide ceramic powder with the particle size of 300-700 nanometers.
Example 4
The method is the same as example 1, except that:
(1) the mass concentration of the hydrochloric acid is 5 percent; the hydrochloric acid accounts for 30 percent of the volume of the water glass, the coupling agent accounts for 10.0 percent of the total volume of the water glass and the hydrochloric acid, and the polyethylene glycol accounts for 5 percent of the total mass of the water glass and the hydrochloric acid; the polymerization degree of the polyethylene glycol is 20000;
(2) the mol ratio of the phenolic resin to the water glass is 10, and the paste is dried at the temperature of 200 ℃ to remove volatile components;
(3) heating the heating furnace to 1550 ℃ and preserving heat for 2 hours to carry out carbothermic reduction reaction;
(4) and (3) preserving the heat of the coarse powder for 2 hours at 650 ℃ to remove residual carbon, cooling the reacted material to normal temperature along with a furnace, and grinding and crushing the cooled material to prepare silicon carbide ceramic powder with the particle size of 350-850 nanometers.
Claims (3)
1. A method for preparing silicon carbide ceramic powder by low-temperature synthesis is characterized by comprising the following steps:
(1) preparing a gel: preparing silicon source water glass, catalyst hydrochloric acid, surfactant coupling agent and polyethylene glycol, wherein the mass concentration of the hydrochloric acid is 5-35%; the hydrochloric acid accounts for 1-30% of the volume of the water glass, the coupling agent accounts for 0.01-10.0% of the total volume of the water glass and the hydrochloric acid, and the polyethylene glycol accounts for 0.01-10.0% of the total mass of the water glass and the hydrochloric acid; sequentially adding water glass, a coupling agent, polyethylene glycol and hydrochloric acid into deionized water, and uniformly stirring to prepare gel; washing the gel with water and alcohol, and filtering to obtain precursor gel; the polymerization degree of the polyethylene glycol is 2000-20000;
(2) preparing precursor powder: putting the precursor gel into absolute ethyl alcohol, adding phenolic resin under the stirring condition, dissolving the phenolic resin in the absolute ethyl alcohol, and dispersing the precursor gel until all materials form a paste; putting the paste body into an oven, drying at 65-200 ℃ to remove volatile components, cooling the residual materials to normal temperature along with the oven, taking out and grinding to prepare precursor powder; wherein the molar ratio of the phenolic resin to the water glass is 0.5-10;
(3) synthesizing: putting the precursor powder into a heating furnace, introducing argon into the heating furnace to remove air, and keeping the argon flowing; then heating the heating furnace to 1400-1550 ℃, preserving heat for 2-5 hours, carrying out carbothermic reduction reaction, and cooling to normal temperature along with the furnace after the reaction is finished to obtain coarse powder;
(4) decarbonization: and (3) placing the coarse powder into a resistance furnace, preserving heat for 2-8 hours at 550-650 ℃ to remove residual carbon, cooling the reacted materials to normal temperature along with the furnace, and grinding to prepare silicon carbide ceramic powder, wherein the particle size of the silicon carbide ceramic powder is 200-1000 nanometers.
2. The method for preparing silicon carbide ceramic powder through low-temperature synthesis according to claim 1, wherein in the step (1), the amount of deionized water is based on the total dissolution of water glass, coupling agent and polyethylene glycol after the deionized water is mixed with hydrochloric acid.
3. The method for preparing silicon carbide ceramic powder through low-temperature synthesis according to claim 1, wherein in the step (2), the absolute ethyl alcohol is used in an amount based on the total dissolution of the phenolic resin.
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Citations (6)
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| JPS56140079A (en) * | 1980-03-28 | 1981-11-02 | Nippon Steel Corp | Indefinite form refractory composition for vibration molding |
| CN101786622A (en) * | 2010-01-20 | 2010-07-28 | 中国科学院山西煤炭化学研究所 | Preparation method of silicon carbide nano-wire |
| CN101804981A (en) * | 2010-04-01 | 2010-08-18 | 中国科学院山西煤炭化学研究所 | Method for preparing hollow silicon carbide nano material |
| CN102432013A (en) * | 2011-10-08 | 2012-05-02 | 中国科学院山西煤炭化学研究所 | Preparation method of beta-nano-SiC |
| CN107963631A (en) * | 2017-12-12 | 2018-04-27 | 宁波爱克创威新材料科技有限公司 | Nanometer silicon carbide and preparation method thereof |
| CN108314050A (en) * | 2018-03-12 | 2018-07-24 | 鲁东大学 | A kind of preparation method of the nanometer silicon carbide particle of efficient absorption organic dyestuff |
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- 2018-12-27 CN CN201811616833.5A patent/CN109437913B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56140079A (en) * | 1980-03-28 | 1981-11-02 | Nippon Steel Corp | Indefinite form refractory composition for vibration molding |
| CN101786622A (en) * | 2010-01-20 | 2010-07-28 | 中国科学院山西煤炭化学研究所 | Preparation method of silicon carbide nano-wire |
| CN101804981A (en) * | 2010-04-01 | 2010-08-18 | 中国科学院山西煤炭化学研究所 | Method for preparing hollow silicon carbide nano material |
| CN102432013A (en) * | 2011-10-08 | 2012-05-02 | 中国科学院山西煤炭化学研究所 | Preparation method of beta-nano-SiC |
| CN107963631A (en) * | 2017-12-12 | 2018-04-27 | 宁波爱克创威新材料科技有限公司 | Nanometer silicon carbide and preparation method thereof |
| CN108314050A (en) * | 2018-03-12 | 2018-07-24 | 鲁东大学 | A kind of preparation method of the nanometer silicon carbide particle of efficient absorption organic dyestuff |
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