Disclosure of Invention
In order to solve the problems in the production and application of silicon carbide, the invention uses SiO2The sol, the polyethylene glycol and the PVA are used as additives, and the preparation method of the SiC ceramic powder is provided.
Specifically, the preparation method of the SiC ceramic powder provided by the invention is implemented according to the following steps:
s1: weighing a certain amount of silicon carbide micro powder, adding the silicon carbide micro powder in S2 into an ethanol aqueous solution under the condition of ultrasonic stirring, continuously stirring for 1-2 hours until the silicon carbide micro powder is fully dispersed, wherein the volume ratio of absolute ethanol to water in the absolute ethanol aqueous solution is 1-3: 1, taking the mass ratio of the volume of the absolute ethyl alcohol to the silicon carbide micro powder as 0.2-1 ml: 1g of a compound;
s2: preparing nano-coated silicon carbide particles;
s21: adding tetraethoxysilane into the SiC mixed solution of S1 under the condition of ultrasonic stirring, wherein SiO contained in the tetraethoxysilane2The mass ratio of the amount of the silicon carbide to the silicon carbide in S1 is 3-10%, continuously stirring, adding glacial acetic acid to adjust the pH value to 1-3, fully reacting for 2-6 h, and drying at 80-120 ℃ for 4-8 h to obtain nano-coated silicon carbide particles;
s3: adding polyethylene glycol 10000 into 10-15 ml of absolute ethyl alcohol under the condition of ultrasonic stirring, wherein the molar ratio of the C content in the polyethylene glycol 10000 to the Si content in ethyl orthosilicate in S21 is 1.2-2, and continuously stirring for 0.5-1 h until the mixture is fully dispersed;
s4, adding the silicon carbide particles coated with the nano particles in the S21 into a mixed solution of S3 polyethylene glycol 10000 under the condition of magnetic stirring, continuously and magnetically stirring for 1-2 hours until the silicon carbide particles are fully dispersed, and drying the mixture for 3-5 hours at 100-150 ℃ to obtain silicon carbide mixed powder;
s5: adding PVA into the silicon carbide mixed powder of S4, wherein the mass percentage of the PVA to the silicon carbide mixed powder of S4 is 3-5%, mechanically stirring for 1-2 h, sealing and standing for 5-10 h after uniform mixing to obtain a SiC micropowder mixture;
s6: pouring the uniformly mixed powder in the S5 into a granulator for granulation to obtain SiC granules with uniform size and granularity ranging from 10 to 200 mu m, and drying the SiC granules at the temperature of 90 to 100 ℃ for 1 to 2 hours to obtain SiC granules with proper humidity;
s7: and (3) putting the silicon carbide particles treated in the step (S6) into a high-temperature vacuum atmosphere furnace for sintering, carrying out heat treatment for 2-3 h at 1300-1500 ℃, cooling to room temperature, putting into a muffle furnace for carrying out heat treatment for 2-3 h at 500-600 ℃, and then obtaining SiC ceramic powder with reconstructed particle size.
Preferably, the particle size of the SiC micropowder used in S1 is 0.5-3 μm.
Preferably, SiO contained in the tetraethoxysilane used in S212The mass ratio of the amount of the silicon carbide to the silicon carbide in the S1 is 3% -10%.
Preferably, the molar ratio of the content of C in polyethylene glycol 10000 used in S3 to the content of Si in tetraethoxysilane used in S21 is 1.2-2, and the organic carbon source polyethylene glycol 10000 can be replaced by polyethylene glycol 2000, polyethylene glycol 6000, polyethylene glycol 20000, glucose and the like.
Preferably, the sintering temperature of the SiC particles in S7 is 1300-1500 ℃, and the sintering atmosphere can be vacuum argon protection and vacuum nitrogen protection; the temperature of the secondary heat treatment is 500-600 ℃.
The silicon carbide ceramic powder with reconstructed granularity prepared by the method has high purity, low porosity and excellent use performance.
The silicon carbide ceramic powder with the reconstructed granularity prepared by the method is widely applied, in particular to the application in the fields of high-temperature corrosion resistance, national defense and military industry, special ceramics and the like.
The technical scheme of the invention has the following beneficial effects:
the invention firstly provides a preparation method of SiC ceramic powder, which utilizes polyethylene glycol 10000 and SiO2The sol and PVA are used as additives, and the problem that the silicon carbide micro powder cannot be utilized due to the excessively fine granularity is solved. Nano SiO2The addition of the sol and the polyethylene glycol 10000 reduces the sintering temperature, and the ceramic powder after particle size reconstruction has high purity, low porosity and excellent service performance, thereby well solving the problem of recycling the waste silicon carbide powder in the aspect of ceramics. The preparation method of the SiC ceramic powder provided by the invention can be well applied to other types of ceramic micro powder, and has good practicability.
Detailed Description
The present invention is further described with reference to the following specific examples, which should be construed by those skilled in the art as being illustrative and not limiting.
All technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In the following examples, unless otherwise specified, the methods used were all conventional methods, and the starting materials used were all commercially available analytical pure materials. Without limiting the invention thereto, one skilled in the art can, in light of the present disclosure and knowledge of the prior art, use similar methods, apparatus, materials to practice the invention repeatedly.
The following specifically exemplifies the technical solution of the present invention.
Example 1
A preparation method of SiC ceramic powder comprises the following specific steps:
s1: weighing 30g of silicon carbide micro powder, adding the silicon carbide micro powder in S2 into 30ml of ethanol aqueous solution under the condition of ultrasonic stirring, and continuously stirring for 2h until the silicon carbide micro powder is fully dispersed, wherein the volume ratio of absolute ethanol to water in the absolute ethanol aqueous solution is 1.5: 1, taking the mass ratio of the volume of the absolute ethyl alcohol to the silicon carbide micro powder as 1 ml: 1g of a compound;
s2: preparing nano-coated silicon carbide particles;
s21: adding tetraethoxysilane into the SiC mixed solution of S1 under the condition of ultrasonic stirring, wherein SiO contained in the tetraethoxysilane2The mass ratio of the amount of the silicon carbide to the silicon carbide in S1 is 5%, the stirring is continued, glacial acetic acid is added to adjust the PH value to 2, the mixture is fully reacted for 6 hours, and the mixture is dried for 8 hours at 80 ℃ to obtain nano-coated silicon carbide particles;
s3: adding polyethylene glycol 10000 into 15ml of absolute ethyl alcohol under the condition of ultrasonic stirring, wherein the molar ratio of the C content in the polyethylene glycol 10000 to the Si content in the tetraethoxysilane in S21 is 1.5, and continuously stirring for 1h until the mixture is fully dispersed;
s4, adding the silicon carbide particles coated with the nano particles in the S21 into a mixed solution of S3 polyethylene glycol 10000 under the condition of magnetic stirring, continuously and magnetically stirring for 2 hours until the silicon carbide particles are fully dispersed, and drying the mixture for 5 hours at 100 ℃ to obtain silicon carbide mixed powder;
s5: adding PVA into the silicon carbide mixed powder of S4, wherein the mass percentage of the PVA to the silicon carbide mixed powder of S4 is 5%, mechanically stirring for 1h, uniformly mixing, sealing and standing for 10h to obtain a SiC micro powder mixture;
s6: pouring the powder uniformly mixed in the S5 into a granulator for granulation to obtain SiC granules with uniform size and granularity of 15 mu m, and drying at 90 ℃ for 1h to obtain SiC granules with proper humidity;
s7: and (3) putting the silicon carbide particles treated in the step (S6) into a high-temperature vacuum atmosphere furnace for sintering, carrying out heat treatment for 3h at 1450 ℃, cooling to room temperature, putting into a muffle furnace for carrying out heat treatment for 2h at 500 ℃, and then obtaining SiC ceramic powder with reconstructed particle size.
Example 2
A preparation method of SiC ceramic powder comprises the following specific steps:
s1: weighing 30g of silicon carbide micro powder, adding the silicon carbide micro powder in S2 into 20ml of ethanol aqueous solution under the condition of ultrasonic stirring, and continuously stirring for 2h until the silicon carbide micro powder is fully dispersed, wherein the volume ratio of absolute ethanol to water in the absolute ethanol aqueous solution is 2: 1, taking the mass ratio of the volume of the absolute ethyl alcohol to the silicon carbide micro powder as 1 ml: 1g of a compound;
s2: preparing nano-coated silicon carbide particles;
s21: adding tetraethoxysilane into the SiC mixed solution of S1 under the condition of ultrasonic stirring, wherein SiO contained in the tetraethoxysilane2The mass ratio of the amount of the silicon carbide to the silicon carbide in S1 is 7%, the stirring is continued, glacial acetic acid is added to adjust the PH value to 3, the mixture is dried for 8 hours at 80 ℃ after the full reaction for 6 hours, and the nano-coated silicon carbide particles are obtained;
s3: adding polyethylene glycol 10000 into 15ml of absolute ethyl alcohol under the condition of ultrasonic stirring, wherein the molar ratio of the C content in the polyethylene glycol 10000 to the Si content in the tetraethoxysilane in S21 is 1.5, and continuously stirring for 1h until the mixture is fully dispersed;
s4, adding the silicon carbide particles coated with the nano particles in the S21 into a mixed solution of S3 polyethylene glycol 10000 under the condition of magnetic stirring, continuously and magnetically stirring for 1h until the silicon carbide particles are fully dispersed, and drying the mixture for 5h at 100 ℃ to obtain silicon carbide mixed powder;
s5: adding PVA into the silicon carbide mixed powder of S4, wherein the mass percentage of the PVA to the silicon carbide mixed powder of S4 is 5%, mechanically stirring for 1h, uniformly mixing, sealing and standing for 10h to obtain a SiC micro powder mixture;
s6: pouring the powder uniformly mixed in the S5 into a granulator for granulation to obtain SiC granules with uniform size and granularity of 20 mu m, and drying at 90 ℃ for 1h to obtain SiC granules with proper humidity;
s7: and (3) putting the silicon carbide particles treated in the step (S6) into a high-temperature vacuum atmosphere furnace for sintering, carrying out heat treatment for 3h at 1450 ℃, cooling to room temperature, putting into a muffle furnace for carrying out heat treatment for 2h at 500 ℃, and then obtaining SiC ceramic powder with reconstructed particle size.
The SiC ceramic powder prepared in the embodiment 1 and the embodiment 2 has the advantages of stable process, reliable quality and excellent performance. For example, SiC ceramic is prepared by selecting SiC particles with the particle sizes of 15 μm and 20 μm prepared in the example 1 and the example 2, and compared with SiC ceramic prepared by SiC powder with the same particle size in the market, the sintering temperature is low; the sintering temperature of the SiC ceramics prepared in the embodiment 1 and the embodiment 2 is respectively reduced by 50 ℃ and 40 ℃, and the strength is respectively improved by 2 percent and 3 percent; the ceramic powder prepared by the invention has good molding fluidity and higher density.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of protection is not limited thereto. The equivalents and modifications of the present invention which may occur to those skilled in the art are within the scope of the present invention as defined by the appended claims.