CN106966732B - Fine powder silicon carbide ceramic and preparation method thereof - Google Patents
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Abstract
The invention discloses a preparation method of fine powder silicon carbide ceramic, and belongs to the technical field of silicon carbide ceramic preparation. Specifically, the silicon carbide ceramic is sintered by taking silicon wafer cutting edge material tailing fine powder as a fine powder raw material through reaction, so that the preparation cost is greatly reduced, impurity removal is carried out on the raw material powder through a chemical method, the raw material silicon carbide fine powder, carbon black, a dispersing agent, a water reducing agent and a dispersing medium are uniformly mixed in a mixer, the mixture is dried after slip casting, and finally high-temperature siliconizing is carried out, so that the refined silicon carbide ceramic with excellent performance is prepared. The preparation method provided by the invention has simple process, takes the fine powder of the silicon wafer cutting edge material tailing with extremely low cost as the fine powder raw material to react and sinter the SiC ceramic, so that the preparation cost is greatly reduced, and the prepared fine powder silicon carbide ceramic has good mechanical property, high density, higher strength, hardness and other excellent properties compared with the common SiC ceramic, and has very wide market space and good economic and social benefits.
Description
Technical Field
The invention belongs to the technical field of silicon carbide ceramic preparation, and particularly relates to a machine for preparing fine powder silicon carbide ceramic by reactive sintering of silicon wafer cutting edge material tailings and a preparation method thereof.
Background
The preparation process of the silicon carbide mainly comprises pressureless sintering and reaction sintering. The pressureless sintering is a process of sintering by adopting inert atmosphere protection and a sintering aid under normal pressure. The elements such as B, Al, Fe, Cr, Ca, Y and the like or oxides thereof are usually used as sintering aids to promote the sintering of the silicon carbideTo densify. The sintering aid is divided into solid phase sintering and liquid phase sintering according to the phase state of the sintering aid in the sintering process. In 1974S Prochazka, high-purity beta-SiC fine powder is used as a raw material, B and C are used as sintering aids, pressureless solid-phase sintering is carried out at 2020 ℃ to prepare silicon carbide ceramic, the density reaches 98%, the bending strength reaches 500MPa, and a sintering mass transfer mode is a diffusion mechanism. Mechanical property research tests show that the product obtained by the process has a transgranular fracture mode, and has the defects of large grain size, poor uniformity and low fracture toughness at high temperature. In addition, the requirement on the purity of raw materials is high, the sintering temperature is more than 2000 ℃, and the energy consumption is overhigh. The liquid phase sintering mechanism is that the sintering aid forms a eutectic liquid phase at the sintering temperature, the sintering mass transfer mode is changed into viscous flow mass transfer, the sintering temperature is reduced, the energy consumption is reduced, and the fracture mode is crystal fracture. Liu Bao Ying and the like adopt 4.5 to 7.5 percent of alumina and 2.5 to 5.5 percent of yttrium oxide as sintering aids, the sintering temperature is 1780 ℃, and the density of the prepared material is 3.13g/cm3And the bending strength reaches 405MPa at room temperature. The liquid phase volatilization can cause the density reduction of the ceramic, so the strength is slightly reduced, and the existence of the liquid phase also influences the high-temperature use performance of the material.
The reactive sintering silicon carbide ceramic directly adopts silicon carbide with certain grain size distribution, the silicon carbide and carbon are mixed to form a green body, then siliconizing is carried out at high temperature, and part of silicon reacts with the carbon to produce the silicon carbide which is combined with the silicon carbide in the original green body, thereby achieving the purpose of sintering. There are two methods of siliconizing: one is that the temperature reaches the melting temperature of silicon to generate a liquid phase of silicon, and the silicon directly enters a blank body to react with carbon to produce silicon carbide through the action of a capillary tube until the silicon is sintered; the other is that the temperature is higher than the melting temperature of silicon, silicon vapor is generated, and the purpose of sintering is achieved by the silicon vapor entering the green body. The residual free silicon after sintering in the former method is generally more, usually reaching 10-15%, sometimes reaching more than 15%; the gas phase method is used for siliconizing, and the content of free silicon after sintering can be reduced to 10 percent because the reserved air holes of the blank body can be reduced as little as possible. Compared with pressureless sintering, reactive sintering can be completed at a lower temperature (1450-1700 ℃), the shrinkage of a sintered product is only within 3%, near-net-size sintering can be realized, and the framework of carbon and silicon carbide can be turned into any shape in advance, which is beneficial to controlling the size and the shape of the product. The adopted raw materials of silicon carbide, C bonding agent and the like do not need special treatment, and the production cost is lower. However, the reaction sintering process determines the residual free silicon in the sintered body, which affects the application of the subsequent product, on one hand, the strength and wear resistance of the sintered body are reduced, and on the other hand, the acid and alkali resistance of the silicon carbide is reduced due to the existence of the free silicon.
Because the reaction sintering production process is relatively simple and the production cost is low, most manufacturers such as silicon carbide sealing elements, silicon carbide bearings, silicon carbide nozzles and the like in China select the reaction sintering production process. However, in the common reaction sintering process, the silicon carbide with particle size distribution is used as a raw material, so that the impurity content is high, and the performance of the reaction sintering material is not high due to wide particle size distribution (10-50 microns). In recent years, partial research adopts nano-grade superfine silicon carbide micro powder as a raw material to prepare the silicon carbide nano-powder with the sintering density of 3.057g/cm3The silicon carbide ceramic with the bending strength of over 800MPa has the microhardness of 28.1 GPa. The mechanical properties of the material are greatly improved, but the nano-scale silicon carbide micro powder raw material is sold at a price of more than ten thousand yuan per ton, the production cost is too high, and the large-scale popularization is not facilitated.
The fine powder SiC ceramic has superior properties such as higher strength and hardness than ordinary SiC ceramics. Because the common reaction sintering SiC ceramic raw material adopts gradation and has wider particle size distribution, the performance is not ideal, and therefore, the exploration of the reaction sintering SiC ceramic prepared by taking the silicon wafer cutting edge tailing fine powder with extremely low cost as the raw material has very wide market space and good economic and social benefits.
Disclosure of Invention
In order to solve the problems in the prior art, the fine powder silicon carbide ceramic is sintered by taking the fine powder of the silicon wafer cutting edge material tailings as a fine powder raw material through reaction, so that the preparation cost is greatly reduced, the impurity of the raw material powder is removed through a chemical method, the raw material silicon carbide fine powder, carbon black and various sintering aids are uniformly mixed in a mixer, and the mixture is dried after slip casting and finally subjected to high-temperature siliconizing to prepare the fine powder silicon carbide ceramic with excellent performance.
Specifically, the preparation method of the fine powder silicon carbide ceramic provided by the invention specifically comprises the following steps:
s1: mixing carbon black, fine powder silicon carbide, a dispersing agent, a water reducing agent and a dispersing medium to obtain mixed slurry, wherein the fine powder silicon carbide is fine powder of a silicon wafer cutting edge material tail material with the particle size of 3.2-3.9 micrometers, and the mass ratio of the carbon black to the fine powder silicon carbide is 1: 6-8, wherein the mass ratio of the dispersing agent to the fine powder silicon carbide is 1: 120-150, wherein the mass ratio of the water reducing agent to the fine powder silicon carbide is 1: 800-1800, wherein the mass ratio of the dispersion medium to the fine powder silicon carbide is 1: 20-25;
s2: performing slip casting on the mixed slurry to obtain a blank, and drying the formed blank at 75-85 ℃ for 4-6 hours;
s3: embedding the dried blank with mixed powder consisting of boron nitride, carbon black and silicon powder, drying at 100-300 ℃ for 2 hours in a vacuum state in sequence, discharging glue at 350-850 ℃ for 3 hours in a nitrogen atmosphere, heating to 1650-1720 ℃ in the vacuum state, and sintering to obtain the fine powder silicon carbide ceramic, wherein the mass ratio of the carbon black to the silicon powder to the boron nitride in the mixed powder is 1: 50: 1000-1250.
Preferably, the dispersing agent is a mixture of polyvinylpyrrolidone-K30 and polyvinylpyrrolidone-K90, and the polyvinylpyrrolidone-K30 and the polyvinylpyrrolidone-K90 in the mixture are mixed according to the mass ratio of 1: 6-12.
Preferably, the water reducing agent is a polycarboxylate water reducing agent CE-64.
Preferably, the dispersion medium is deionized water.
Preferably, in S1, the step of mixing the carbon black, the fine powder of silicon carbide, the dispersant, the water reducing agent and the dispersion medium to obtain the mixed slurry comprises: adding carbon black, fine powder silicon carbide, a dispersing agent and a water reducing agent into a dispersion medium, stirring for 4-5 hours, and testing the viscosity to be less than or equal to 800mPa.s at room temperature.
Preferably, the sintering step in S3 is: the sintering step in S3 is: and drying the embedded blank for 2 hours at 150-200 ℃ in a vacuum state, removing glue for 3 hours at 560-600 ℃ in a nitrogen atmosphere, heating to 1650-1720 ℃ in the vacuum state, sintering, keeping the temperature for 2 hours, and cooling to room temperature along with the furnace temperature.
The invention also provides fine powder silicon carbide ceramic prepared by any one of the preparation methods.
Preferably, the density of the silicon carbide ceramic is 3.03-3.05 g/cm3The bending strength is 550 to 580 MPa.
The preparation method of the fine powder silicon carbide ceramic provided by the invention is simple in process, takes the fine powder of the silicon wafer cutting edge material tailing with extremely low cost as a fine powder raw material to react and sinter the SiC ceramic, so that the preparation cost is greatly reduced, a mixture of polyvinylpyrrolidone-K30 and polyvinylpyrrolidone-K90 is selected as a dispersing agent, and a polycarboxylate water reducer CE-64 is selected as a water reducer, so that the fine powder silicon carbide ceramic has a good dispersing effect on the silicon wafer cutting edge material tailing with the particle size of 3.2-3.9 micrometers; the blank is embedded by using mixed powder consisting of boron nitride, carbon black and silicon powder, so that the content of free silicon in the final product is controlled, the mechanical property of the product is enhanced, and the maximum use temperature of the product is increased; the prepared fine powder silicon carbide ceramic has good mechanical property and high density, has excellent properties of higher strength, hardness and the like compared with common SiC ceramic, and has very wide market space and good economic and social benefits.
Drawings
FIG. 1 is a flow chart of a method for preparing a fine powder silicon carbide ceramic according to an embodiment of the present invention;
fig. 2 is a fracture scanning picture of the fine powder silicon carbide ceramic provided in example 2 of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood and enable those skilled in the art to practice the present invention, the following embodiments are further described, but the present invention is not limited to the following embodiments.
A preparation method of fine powder silicon carbide ceramic is shown in figure 1 and comprises the following steps:
s1: mixing carbon black, fine powder silicon carbide, a dispersing agent, a water reducing agent and a dispersing medium to obtain mixed slurry, wherein the fine powder silicon carbide is fine powder of silicon wafer cutting edge material tails with the particle size of 3.2-3.9 micrometers, and the mass ratio of the carbon black to the fine powder silicon carbide is 1: 6-8, wherein the mass ratio of the dispersing agent to the fine powder silicon carbide is 1: 120-150, wherein the mass ratio of the water reducing agent to the fine powder silicon carbide is 1: 800-1800, wherein the mass ratio of the dispersion medium to the fine powder silicon carbide is 1: 20-25;
s2: performing slip casting on the mixed slurry to obtain a blank, and drying the formed blank at 75-85 ℃ for 4-6 hours;
s3: embedding the dried blank with mixed powder consisting of boron nitride, carbon black and silicon powder, sequentially heating to 100-300 ℃ at a speed of 5 ℃/min in a vacuum state for drying for 2 hours, heating to 350-850 ℃ at a speed of 5 ℃/min in a nitrogen atmosphere for binder removal for 3 hours, heating to 1650-1720 ℃ at a speed of 5 ℃/min in a vacuum state for sintering, keeping the temperature for 2 hours, and cooling to room temperature along with the furnace temperature to obtain the fine powder silicon carbide ceramic, wherein the mass ratio of the carbon black, the silicon powder and the boron nitride in the mixed powder is 1: 50: 1000-1250.
The SiC ceramic is prepared by reaction sintering of silicon wafer cutting edge material tailing fine powder serving as a fine powder raw material, the preparation cost is greatly reduced, impurity removal is carried out on the raw material powder through a chemical method, the raw material silicon carbide fine powder, carbon black and various sintering aids are uniformly mixed in a mixer, the mixture is dried after slip casting, and finally high-temperature siliconizing is carried out, so that the high-density fine-particle reaction sintered silicon carbide ceramic is obtained.
Because the grain diameter of the silicon wafer cutting edge material tailing as raw material powder is 3.2-3.9 microns, the silicon wafer cutting edge material tailing is difficult to disperse, and the uniform slurry preparation by selecting a dispersing agent and a water reducing agent is a technical difficulty for preparing silicon carbide ceramics, the dispersing agent adopts polyvinylpyrrolidone, preferably, a mixture of polyvinylpyrrolidone-K30 and polyvinylpyrrolidone-K90 in a certain proportion is selected, and the requirements of viscosity and strength in a system are met through the combined adjustment of polymerization degrees; the water reducing agent is selected from a polycarboxylate water reducing agent CE-64 to reduce viscosity and increase stability, so that the silicon wafer cutting edge material tailing material is well dispersed, and uniform mixed slurry is obtained; because the content of free silicon in the target product has great influence on the mechanical property and the maximum use temperature of the product, the blank is embedded by the mixed powder consisting of boron nitride, carbon black and silicon powder in the preparation process so as to control the content of free silicon in the final product and enhance the mechanical property of the product.
The preparation of fine silicon carbide ceramics by the preparation method of the present invention will be specifically exemplified below.
Example 1
A preparation method of fine powder silicon carbide ceramic comprises the following steps:
adding 140g of carbon black, 860g of fine powder silicon carbide with the particle size of 3.2 microns, 6g of polyvinylpyrrolidone-K90, 0.5g of polyvinylpyrrolidone-K30 and 0.5g of polycarboxylic acid water reducing agent CE-64 into 40g of deionized water, mechanically stirring for 5 hours, uniformly mixing, and testing the viscosity at room temperature by using a rotational viscometer to be not higher than 800mPa.s to obtain mixed slurry;
performing slip casting on the mixed slurry to obtain a blank, and drying the formed blank in an oven at 80 ℃ for 5 hours; embedding the dried sample by using boron nitride carbon black mixed powder with silicon content of 70g, wherein the mixed powder consists of 1.4g of carbon black, 70g of silicon powder and 1400g of boron nitride. Placing the mixture in a sintering furnace, sequentially heating to 150 ℃ at a speed of 5 ℃/min under a vacuum state, drying for 2 hours, heating to 600 ℃ at a speed of 5 ℃/min under a nitrogen atmosphere, discharging glue for 3 hours, heating to 1700 ℃ at a speed of 5 ℃/min under a vacuum state, sintering, keeping the temperature for 2 hours, cooling to room temperature along with the furnace temperature, taking out a sample, and polishing to obtain a final product. The density of the final sample was 3.05g/cm3The flexural strength was 580 MPa.
Example 2
A preparation method of fine powder silicon carbide ceramic comprises the following steps:
adding 140g of carbon black, 860g of fine powder silicon carbide with the particle size of 3.6 microns, 6g of polyvinylpyrrolidone-K90, 1g of polyvinylpyrrolidone-K30 and 0.5g of polycarboxylic acid water reducing agent CE-64 into 36g of deionized water, mechanically stirring for 5 hours, uniformly mixing, and testing the viscosity at room temperature by using a rotational viscometer to be not higher than 700mPa.s to obtain mixed slurry;
performing slip casting on the mixed slurry to obtain a blank, and drying the formed blank in an oven at 80 ℃ for 5 hours; embedding the dried sample by using boron nitride carbon black mixed powder with the silicon content of 80g, wherein the mixed powder consists of 1.6g of carbon black, 80g of silicon powder and 1920g of boron nitride. Placing the mixture into a sintering furnace, sequentially heating to 150 ℃ at a speed of 5 ℃/min under a vacuum state, drying for 2 hours, heating to 600 ℃ at a speed of 5 ℃/min under a nitrogen atmosphere, discharging glue for 3 hours, heating to 1700 ℃ at a speed of 5 ℃/min under a vacuum state, sintering, keeping the temperature for 2 hours, cooling to room temperature along with the furnace temperature, taking out a sample, and grinding to obtain a final product. The density of the final sample was 3.03g/cm3The flexural strength was 550 MPa.
Example 3
A preparation method of fine powder silicon carbide ceramic comprises the following steps:
adding 140g of carbon black, 860g of fine powder silicon carbide with the particle size of 3.9 microns, 6g of polyvinylpyrrolidone-K90, 1g of polyvinylpyrrolidone-K30 and 0.5g of polycarboxylic acid water reducing agent CE-64 into 36g of deionized water, mechanically stirring for 5 hours, uniformly mixing, and testing the viscosity at room temperature by using a rotational viscometer to be not higher than 700mPa.s to obtain mixed slurry;
performing slip casting on the mixed slurry to obtain a blank, and drying the formed blank in an oven at 85 ℃ for 5 hours; embedding the dried sample by using boron nitride carbon black mixed powder with the silicon content of 80g, wherein the mixed powder consists of 1.6g of carbon black, 80g of silicon powder and 1760g of boron nitride. And placing the mixture into a sintering furnace, sequentially heating to 200 ℃ at a speed of 5 ℃/min in a vacuum state, drying for 2 hours, heating to 580 ℃ at a speed of 5 ℃/min in a nitrogen atmosphere, discharging glue for 3 hours, heating to 1650 ℃ at a speed of 5 ℃/min in a vacuum state, sintering, keeping the temperature for 2 hours, cooling to room temperature along with the furnace temperature, taking out a sample, and grinding to obtain a final product. The density of the final sample was 3.06g/cm3The flexural strength was 570 MPa.
The fine powder silicon carbide ceramic prepared in example 2 was subjected to SEM test and bending strength test, and the sintered sample was taken out and sampled into a 3 × 3 × 36mm long strip, subjected to three-point bending strength test in a universal testing machine, and then observed for fracture morphology under a scanning electron microscope. The fracture morphology of the sample obtained in example 2 is shown in FIG. 2. The figure shows that the size of the silicon carbide particles is about 3.6 microns, larger air hole distribution is not found, the structure is uniform, and the three-point bending strength test shows that the bending strength reaches 550MPa, which is closely related to the high density and the small air hole content.
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.
Claims (4)
1. The preparation method of the fine powder silicon carbide ceramic is characterized by comprising the following steps:
s1: mixing carbon black, fine powder silicon carbide, a dispersing agent, a water reducing agent and a dispersion medium to obtain mixed slurry, wherein the dispersing agent is a mixture of polyvinylpyrrolidone-K30 and polyvinylpyrrolidone-K90, the polyvinylpyrrolidone-K30 and the polyvinylpyrrolidone-K90 in the mixture are mixed according to a mass ratio of 1: 6-12, the water reducing agent is a polycarboxylic acid water reducing agent CE-64, the dispersion medium is deionized water, the fine powder silicon carbide is fine powder of silicon wafer cutting edge material tailings with the particle size of 3.2-3.9 microns, and the mass ratio of the carbon black to the fine powder silicon carbide is 1: 6-8, wherein the mass ratio of the dispersing agent to the fine powder silicon carbide is 1: 120-150, wherein the mass ratio of the water reducing agent to the fine powder silicon carbide is 1: 800-1800, wherein the mass ratio of the dispersion medium to the fine powder silicon carbide is 1: 20-25;
s2: performing slip casting on the mixed slurry to obtain a blank, and drying the formed blank at 75-85 ℃ for 4-6 hours;
s3: embedding the dried blank with mixed powder consisting of boron nitride, carbon black and silicon powder, drying the embedded blank for 2 hours at 150-200 ℃ in a vacuum state, discharging glue for 3 hours at 560-600 ℃ in a nitrogen atmosphere, heating to 1650-1720 ℃ in the vacuum state, sintering, keeping the temperature for 2 hours, and cooling to room temperature along with the furnace temperature to obtain the fine powder silicon carbide ceramic, wherein the mass ratio of the carbon black, the silicon powder and the boron nitride in the mixed powder is 1: 50: 1000-1250.
2. The method for preparing the fine powder silicon carbide ceramic according to claim 1, wherein in S1, the specific steps of mixing the carbon black, the fine powder silicon carbide, the dispersant, the water reducing agent and the dispersion medium to obtain the mixed slurry are as follows:
adding carbon black, fine powder silicon carbide, a dispersing agent and a water reducing agent into a dispersion medium, stirring for 4-5 hours, and testing the viscosity to be less than or equal to 800mPa.s at room temperature.
3. A fine powder silicon carbide ceramic produced by the production method according to any one of claims 1 to 2.
4. The fine powder silicon carbide ceramic according to claim 3, wherein the fine powder silicon carbide ceramic has a density of 3.03 to 3.05g/cm3The bending strength is 550 to 580 MPa.
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| CN112174675A (en) * | 2020-10-21 | 2021-01-05 | 上海德宝密封件有限公司 | Preparation method of reaction sintering silicon carbide |
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