CN107673761B - Preparation method of large-size compact silicon carbide ceramic plate - Google Patents
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Abstract
The invention discloses a preparation method of a large-size compact silicon carbide ceramic plate, which relates to the technical field of reaction sintering of silicon carbide ceramic, and comprises the steps of material mixing, spray granulation, hot press molding, humidification drying, processing, high-temperature drying and reaction sintering, wherein silicon carbide proportioning is used in a supernormal way, humidification drying is carried out after spray granulation and hot press molding, silicon powder with the weight of 200-300% of that of a blank body is added during reaction sintering, and an oxygen-free environment is kept, so that the sintered silicon carbide ceramic plate is not cracked, compact and uniform in density, and high in yield, technical obstacles in sintering of large-size silicon carbide ceramic plates with the length of 600-800 mm, the width of 400-600 mm and the thickness of 40-60 mm are solved, domestic blank is filled, import is successfully replaced, and use cost in the application field is reduced.
Description
Technical Field
The invention relates to a preparation method of a silicon carbide ceramic plate, in particular to a preparation method of a large-size compact silicon carbide ceramic plate with the length of 600-800 mm, the width of 400-600 mm and the thickness of 40-60 mm, and belongs to the technical field of silicon carbide ceramics.
Background
The silicon carbide ceramic has the excellent characteristics of high-temperature strength, strong oxidation resistance, good wear resistance, good thermal stability, small thermal expansion coefficient, high thermal conductivity, high hardness, thermal shock resistance, chemical corrosion resistance and the like, and the high-temperature mechanical properties (strength, creep resistance and the like) are the best in the known ceramic materials, so that the silicon carbide ceramic is more and more widely applied, and the tentacles of the silicon carbide ceramic almost extend to all industrial fields, play more and more important roles in the material field and are increasingly paid more attention by people.
According to different industrial fields and different working conditions and use environments, silicon carbide materials can be used for manufacturing different types of silicon carbide ceramic structural parts by various processes so as to meet application requirements. However, for the structural characteristics of the large-size silicon carbide ceramic plate, such as ultra-long, ultra-wide and ultra-thick, the preparation of the large-size silicon carbide ceramic plate meets technical obstacles of formulation, forming, drying, firing and the like, and particularly, the problems of cracking, uneven density, poor compactness, raw firing and the like are very easy to occur, so that the large-size silicon carbide ceramic plate becomes a technical difficulty and a manufacturing blank in the industry.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a large-size compact silicon carbide ceramic plate, and particularly ensures that the plate is not cracked, compact, uniform in density and high in yield when the silicon carbide ceramic plate with the length of 600-800 mm, the width of 400-600 mm and the thickness of 40-60 mm is prepared.
The technical scheme adopted by the invention is as follows: a preparation method of a large-size compact silicon carbide ceramic plate is provided, wherein the length of the silicon carbide ceramic plate is 600-800 mm, the width of the silicon carbide ceramic plate is 400-600 mm, and the thickness of the silicon carbide ceramic plate is 40-60 mm, and the preparation method comprises the following steps:
1) mixing materials: mixing 1-2 parts by weight of graphite powder with the purity of 99.8-99.9% and 25-30 parts by weight of silicon carbide powder with the purity of 99.8-99.9%, adding 2-4 parts by weight of zinc stearate and 15-20 parts by weight of polyvinyl alcohol, and uniformly stirring to obtain a mixture;
2) spray granulation: spraying and granulating the mixture by using a centrifugal spray dryer to obtain granulated powder;
3) hot-press molding: loading the prepared granulated powder into a metal die, and pressurizing and releasing the pressure for 4-5 times by using a 500-600T hot press at the temperature of 180-200 ℃ and the pressure of 35-55 MPa to obtain a blank of a hot-press molded plate;
4) and (3) humidifying and drying: placing the molded blank body in humidifying and drying equipment, and slowly humidifying and drying for 100-120 hours at the temperature of 30-50 ℃ and the humidity of 40-60%;
5) processing and modifying: carrying out corresponding processing treatment on the dried blank by using mechanical processing equipment to finish the plate with the required accurate geometric shape;
6) and (3) high-temperature drying: placing the processed blank body in a high-temperature drying chamber, and drying for 40-60 hours at the temperature of 100-120 ℃;
7) reaction sintering: arranging a plurality of blanks dried at high temperature on a burning support in parallel, wherein the distance between the blanks arranged on the burning support in parallel is 50-100 mm, adding metal silicon powder with the weight of 200-300% and the purity of 98-99% of the blanks, and putting the blanks into a vacuum electric furnace; after the electric furnace is powered on, in a vacuum state, heating the temperature from room temperature to 1900-2100 ℃ for 40-60 hours, and keeping the temperature for 8-10 hours; then, charging helium gas for rapidly cooling to 300 ℃ within 10-20 hours; heating again, heating from 300 ℃ to 1400-1600 ℃ for 5-10 hours, and keeping the temperature for 5-7 hours; and cooling for 30-50 hours to 100 ℃, stopping power transmission, naturally cooling to room temperature, and discharging to obtain the silicon carbide ceramic plate.
After the technical scheme is adopted, the invention has the beneficial effects that:
1) the content of silicon carbide is increased in the mixture ratio by a supernormal way, and tests prove that the density of a blank is increased, and the compactness of a sintered body is improved.
2) The granulated powder after spray granulation is hot-pressed and molded, and the contact and diffusion among blank powder particles are facilitated by pressurization at high temperature, so that the sintering temperature is reduced, the sintering time is shortened, and the molding is easier.
3) The method comprises the steps of slowly humidifying and drying a biscuit of the silicon carbide ceramic plate in a humidifying and drying device, and then drying the biscuit at a high temperature and performing reaction sintering, so that the problems that the surface moisture of the biscuit is evaporated too fast and is not adaptive to the internal moisture diffusion of the biscuit, the internal and external moisture of the biscuit is uneven, and the biscuit is easy to crack and deform in the traditional drying mode can be effectively solved.
4) In the sintering step, the amount of metal silicon powder accounting for 200-300% of the weight of the blank is added, and the first heating and cooling sintering process is carried out, so that the strength and density of the blank are increased, and the compactness of a sintered body is improved; the rapid cooling can be realized by filling helium; the second heating and cooling sintering process avoids the problem of raw sintering, and simultaneously detects the change state of the sintered body in a high-temperature state to ensure the sintering quality. The sintering process is carried out in an oxygen-free environment, and tests prove that the sintering process is important for improving the compactness of a sintered body and reducing plate cracking.
5) The boards are arranged on the burning frame in parallel at a distance of 50-100 mm, so that the burning space can be fully utilized, the loading capacity of the boards is increased, and the production efficiency is improved.
In conclusion, according to the preparation method disclosed by the invention, silicon carbide proportioning is used in a supernormal way, the silicon powder accounting for 200-300% of the weight of the blank is added and an anaerobic environment is kept during reactive sintering, so that the sintered silicon carbide ceramic plate is prevented from cracking, is compact and uniform in density, has a high yield, solves the technical obstacles in sintering large-size silicon carbide ceramic plates with the length of 600-800 mm, the width of 400-600 mm and the thickness of 40-60 mm, fills up the domestic blank, successfully replaces the import, and reduces the use cost in the application field.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
A silicon carbide ceramic plate having a length X a width X a thickness of 600mm X400 mm X40 mm was prepared by the following method comprising the steps of:
1) mixing materials: mixing 1 part by weight of graphite powder with the purity of 99.8-99.9% and 25 parts by weight of silicon carbide powder with the purity of 99.8-99.9%, adding 2 parts by weight of zinc stearate and 15 parts by weight of polyvinyl alcohol, and uniformly stirring to obtain a mixture;
2) spray granulation: spraying and granulating the mixture by using a centrifugal spray dryer to obtain granulated powder;
3) hot-press molding: loading the prepared granulated powder into a metal die, and pressurizing and releasing the pressure for 4 times by adopting a 500-600T hot press under the conditions of 180 ℃ and 35MPa to obtain a blank of a hot-press molding plate;
4) and (3) humidifying and drying: placing the formed blank body in a humidifying and drying device, and slowly humidifying and drying for 100 hours at the temperature of 30 ℃ and the humidity of 40%;
5) processing and modifying: carrying out corresponding processing treatment on the dried blank by using mechanical processing equipment to finish the plate with the required accurate geometric shape;
6) and (3) high-temperature drying: placing the processed blank body in a high-temperature drying chamber, and drying for 40 hours at the temperature of 100 ℃;
7) reaction sintering: arranging a plurality of high-temperature dried blanks on a burning support in parallel at a distance of 100mm, adding metal silicon powder with the weight of 300% of the blanks and the purity of 98-99%, and putting the metal silicon powder into a vacuum electric furnace; after the electric furnace is powered on, in a vacuum state, the temperature is raised to 1900 ℃ from room temperature for 40 hours, and then the temperature is kept for 8 hours; then, charging helium to quickly cool to 300 ℃ within 10 hours; heating again, and heating from 300 ℃ to 1400 ℃ for 5 hours, and keeping the temperature for 5 hours; and cooling to 100 ℃ within 30 hours, stopping power transmission, naturally cooling to room temperature, and discharging to obtain the silicon carbide ceramic plate.
Example 2
A silicon carbide ceramic plate having a length x width x thickness of 700mm x 500mm x 50mm was prepared by the following method comprising the steps of:
1) mixing materials: mixing 1.4 parts by weight of graphite powder with the purity of 99.8-99.9% and 28 parts by weight of silicon carbide powder with the purity of 99.8-99.9%, adding 3 parts by weight of zinc stearate and 18 parts by weight of polyvinyl alcohol, and uniformly stirring to obtain a mixture;
2) spray granulation: spraying and granulating the mixture by using a centrifugal spray dryer to obtain granulated powder;
3) hot-press molding: loading the prepared granulated powder into a metal die, and pressurizing and releasing the pressure for 5 times by adopting a 500-600T hot press under the conditions of the temperature of 190 ℃ and the pressure of 45MPa to obtain a blank of a hot-press molding plate;
4) and (3) humidifying and drying: placing the formed blank body in a humidifying and drying device, and slowly humidifying and drying for 110 hours at the temperature of 40 ℃ and the humidity of 50%;
5) processing and modifying: carrying out corresponding processing treatment on the dried blank by using mechanical processing equipment to finish the plate with the required accurate geometric shape;
6) and (3) high-temperature drying: placing the processed blank body in a high-temperature drying chamber, and drying for 50 hours at the temperature of 110 ℃;
7) reaction sintering: arranging a plurality of high-temperature dried blanks on a burning support in parallel at a distance of 70mm, adding metal silicon powder with the weight of 250% of the blanks and the purity of 98-99%, and putting the metal silicon powder into a vacuum electric furnace; after the electric furnace is powered on, in a vacuum state, the temperature is raised to 2000 ℃ from room temperature within 50 hours, and then the temperature is kept for 9 hours; then, charging helium to quickly cool to 300 ℃ within 15 hours; heating again, and heating from 300 ℃ to 1500 ℃ for 8 hours, and keeping the temperature for 6 hours; and cooling to 100 ℃ within 40 hours, stopping power transmission, naturally cooling to room temperature, and discharging to obtain the silicon carbide ceramic plate.
Example 3
A silicon carbide ceramic plate having a length x width x thickness of 800mm x 600mm x 60mm was prepared by the following method comprising the steps of:
1) mixing materials: mixing 2 parts by weight of graphite powder with the purity of 99.8-99.9% and 30 parts by weight of silicon carbide powder with the purity of 99.8-99.9%, adding 4 parts by weight of zinc stearate and 20 parts by weight of polyvinyl alcohol, and uniformly stirring to obtain a mixture;
2) spray granulation: spraying and granulating the mixture by using a centrifugal spray dryer to obtain granulated powder;
3) hot-press molding: loading the prepared granulated powder into a metal die, and pressurizing and releasing pressure by adopting a 500-600T hot press under the conditions of 200 ℃ and 55MPa to obtain a blank of a hot-press molding plate;
4) and (3) humidifying and drying: placing the formed blank body in a humidifying and drying device, and slowly humidifying and drying for 120 hours at the temperature of 50 ℃ and the humidity of 60%;
5) processing and modifying: carrying out corresponding processing treatment on the dried blank by using mechanical processing equipment to finish the plate with the required accurate geometric shape;
6) and (3) high-temperature drying: placing the processed blank body in a high-temperature drying chamber, and drying for 60 hours at the temperature of 120 ℃;
7) reaction sintering: arranging a plurality of blanks dried at high temperature on a burning support in parallel, adding metal silicon powder with the weight of 200% of the blanks and the purity of 98-99%, and filling the metal silicon powder into a vacuum electric furnace; after the electric furnace is powered on, in a vacuum state, the temperature is raised to 2100 ℃ from room temperature for 60 hours, and then the temperature is kept for 10 hours; then, charging helium to rapidly cool to 300 ℃ within 20 hours; heating again, and heating from 300 ℃ to 1600 ℃ for 10 hours, and keeping the temperature for 7 hours; and cooling to 100 ℃ within 50 hours, stopping power transmission, naturally cooling to room temperature, and discharging to obtain the silicon carbide ceramic plate.
The main steps of the above examples and comparative examples and the performance parameters of the sintered ceramic slabs are shown in the following table:
| example 1 | Example 2 | Example 3 | Comparative example | |
| During mixing, the proportion of graphite powder and silicon carbide | 1:25 | 1:20 | 1:15 | 1:5 |
| After mixing, spray granulation, hot press molding, humidification and drying | Is that | Is that | Is that | Ordinary dry pressing |
| The proportion of the blank to the added metal silicon powder during reaction sintering | 1:3 | 1:2.5 | 1:2 | 1:0.4 |
| Reaction sintering environment | Primary vacuum sintering and secondary vacuum sintering | Primary vacuum sintering and secondary vacuum sintering | Primary vacuum sintering and secondary vacuum sintering | Vacuum sintering and oxidation sintering |
| Density (g/cm)3) | 3.10 | 3.08 | 3.07 | 3.04 |
| Crack(s) | Is free of | Is free of | Is free of | Has micro cracks |
The present invention is not limited to the specific embodiments described above, which do not contribute to the prior art by a certain step and a certain parameter, but by a combination of these steps and process parameters, and which are not obtainable by a limited number of experiments, some of which use extraordinary settings, such as: the ratio of the graphite powder to the silicon carbide is generally considered to be 1: 2-5, the ratio of the graphite powder to the silicon carbide is 1-2: 25-30, meanwhile, in the reaction sintering step, the using amount of the metal silicon powder is increased, the ratio of the blank to the metal silicon powder is generally considered to be reasonable in the range of 1: 0.3-0.4, but the ratio of 1: 2-3 is adopted in the application, so that the technical obstacle of ordinary technicians in the field in preparing large-size silicon carbide ceramic plates with the length of 600-800 mm, the width of 400-600 mm and the thickness of 40-60 mm is solved, the sintered ceramic plates are guaranteed not to crack, compact and uniform in density, the finished product rate is high, the domestic blank is filled, the import is replaced, and the use cost of the application field is reduced.
Claims (1)
1. A preparation method of a large-size compact silicon carbide ceramic plate is characterized by comprising the following steps of:
1) mixing materials: mixing 1-2 parts by weight of graphite powder with the purity of 99.8-99.9% and 25-30 parts by weight of silicon carbide powder with the purity of 99.8-99.9%, adding 2-4 parts by weight of zinc stearate and 15-20 parts by weight of polyvinyl alcohol, and uniformly stirring to obtain a mixture;
2) spray granulation: spraying and granulating the mixture by using a centrifugal spray dryer to obtain granulated powder;
3) hot-press molding: loading the prepared granulated powder into a metal die, and pressurizing and releasing the pressure for 4-5 times by using a 500-600T hot press at the temperature of 180-200 ℃ and the pressure of 35-55 MPa to obtain a blank of a hot-press molded plate;
4) and (3) humidifying and drying: placing the molded blank body in humidifying and drying equipment, and slowly humidifying and drying for 100-120 hours at the temperature of 30-50 ℃ and the humidity of 40-60%;
5) processing and modifying: carrying out corresponding processing treatment on the dried blank by using mechanical processing equipment to finish the plate with the required accurate geometric shape;
6) and (3) high-temperature drying: placing the processed blank body in a high-temperature drying chamber, and drying for 40-60 hours at the temperature of 100-120 ℃;
7) reaction sintering: arranging a plurality of blanks dried at high temperature on a burning support in parallel, wherein the distance between the blanks arranged on the burning support in parallel is 50-100 mm, adding metal silicon powder with the weight of 200-300% and the purity of 98-99% of the blanks, and putting the blanks into a vacuum electric furnace; after the electric furnace is powered on, in a vacuum state, heating the temperature from room temperature to 1900-2100 ℃ for 40-60 hours, and keeping the temperature for 8-10 hours; then, charging helium gas for rapidly cooling to 300 ℃ within 10-20 hours; heating again, heating from 300 ℃ to 1400-1600 ℃ for 5-10 hours, and keeping the temperature for 5-7 hours; and cooling for 30-50 hours to 100 ℃, stopping power transmission, naturally cooling to room temperature, and discharging to obtain the silicon carbide ceramic plate.
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| CN113956046A (en) * | 2021-10-18 | 2022-01-21 | 浙江东新新材料科技有限公司 | Pressureless sintering silicon carbide large-diameter bearing disc and preparation method thereof |
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