CN115368143A - Silicon nitride microcrystal plate and its production process - Google Patents
Silicon nitride microcrystal plate and its production process Download PDFInfo
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Abstract
The invention provides a silicon nitride microcrystalline plate and a production process thereof, and relates to the technical field of production processes of silicon nitride microcrystalline plates. The silicon nitride microcrystal plate and the production process thereof have the composition that coarse, medium and fine particles SIC containing SIC more than 98 percent and industrial silicon powder containing SIC more than 98 percent, particles less than 10 mu m and particles with the maximum size not more than 20 mu m are used as raw materials, and the method comprises the following steps: s1, preparing coarse, medium and fine particles SIC containing SIC more than 98% and industrial silicon powder containing SIC more than 98%, particles smaller than 10 microns and particles not larger than 20 microns at most, and blending to obtain a mixed material. On the basis of controlling raw materials required by the production of the silicon nitride microcrystalline plate, each production process flow of the silicon nitride microcrystalline plate from material preparation, material mixing, molding, drying, sintering and detection is strictly controlled, so that the sintering difficulty is reduced, unstable variable factors existing in the production process are greatly avoided, and the yield-increasing benefit and the energy-saving and consumption-reducing benefit are favorably improved.
Description
Technical Field
The invention relates to the technical field of a silicon nitride microcrystalline plate production process, in particular to a silicon nitride microcrystalline plate and a production process thereof.
Background
The silicon nitride microcrystal plate is formed by main raw materials such as boron nitride, zirconium oxide, silicon carbide, silicon nitride and the like, the raw materials are pressed and formed into a blank body, and the blank body is dried and then made into a material with high wear resistance, high temperature resistance and high thermal shock stability under the high-temperature environment of a repeated sintering process.
In the production process of the silicon nitride microcrystal plate, because Si3N4 and SiC have similar crystal structures and are covalent bonded compounds, sintering is difficult, unstable variable factors also exist in the production process, and if the process flow of each stage from the selection of the raw materials of the silicon nitride microcrystal plate to the detection of the yield is not strictly controlled, the yield increasing benefit and the energy saving and consumption reducing benefit cannot be improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the silicon nitride microcrystalline plate and the production process thereof, which solve the problems that the silicon nitride microcrystalline plate is difficult to sinter, and the yield increasing benefit and the energy saving and consumption reducing benefit cannot be improved.
In order to achieve the purpose, the invention is realized by the following technical scheme: the silicon nitride microcrystal plate consists of coarse, medium and fine SiC grains with SiC content greater than 98% and industrial silicon powder with Si content greater than 98%, grain size smaller than 10 micron and grain size not greater than 20 micron as material.
Preferably, the production process of the silicon nitride microcrystalline plate comprises the following steps:
s1, preparing coarse, medium and fine SiC particles containing more than 98% of SiC and industrial silicon powder containing more than 98% of Si, less than 10 mu m and no more than 20 mu m at most, and mixing to obtain a mixed material;
s2, placing particles in the raw materials into a mixer for mixing for 3 minutes, slowly pouring weighed water and water-soluble binding agent into the mixer for mixing for 5 minutes according to a proportion so that the particles in the raw materials can fully absorb water, adding powdery raw materials and the binding agent after mixing for 5 minutes, mixing for 15 minutes to complete mixing, pouring the mixture into a skip car for standing, performing secondary mixing after standing, and pulling the mixed mixture to a forming workshop for forming;
s3, pouring the weighed raw materials into the mold, and simultaneously forming under the pressure of 19.6 MPa;
s4, placing the semi-finished bricks into the porous metal drying plate, naturally drying the semi-finished bricks in the shade, and conveying the semi-finished bricks into a drying kiln for drying after the semi-finished bricks are naturally dried in the shade;
s5, placing the dried product into the kiln, adjusting the sintering control temperature, performing nitridation sintering treatment on the dried product, and naturally cooling after sintering to obtain a finished product.
Preferably, in the second S2 step, the mixing ratio of water to the water-soluble binder is 2. .
Preferably, in the step S4, the drying temperature in the drying kiln is 150-500 ℃, and the heat preservation temperature is 180 ℃.
Preferably, in the step S5, the firing temperature of the firing treatment is 800 ℃ to 1800 ℃, and the heat preservation temperature is 800 ℃ to 1350 ℃.
Preferably, in the step S5, the product is naturally cooled to 200 ℃ to 210 ℃ below zero after the product is fired.
Preferably, in the step S5, the color of the product after nitriding and firing is off-white or light yellow, and the surface of the product does not show glass gloss, and the product is acceptable.
The invention provides a silicon nitride microcrystalline plate and a production process thereof. The method has the following beneficial effects:
according to the invention, on the basis of controlling raw materials required by the production of the silicon nitride microcrystalline plate, the silicon nitride microcrystalline plate is strictly controlled from each production process flow of material preparation, material mixing, molding, drying, sintering and detection, and corresponding standards are established at the same time, so that the silicon nitride microcrystalline plate raw materials can sequentially pass through each step after meeting the standards and are finally prepared into a finished product, the sintering difficulty of the silicon nitride microcrystalline plate is reduced, unstable variable factors in the production process are greatly avoided, and the yield increase benefit, the energy saving and the consumption reduction benefit of the silicon nitride microcrystalline plate are favorably improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b):
the embodiment of the invention provides a silicon nitride microcrystal plate, which comprises coarse, medium and fine SiC particles containing more than 98% of SiC and industrial silicon powder containing more than 98% of Si, particles smaller than 10 mu m and particles with the maximum size of no more than 20 mu m as raw materials, wherein the purchase of the raw materials needs strict control, the SiC content in the silicon carbide raw materials is not less than 98.5%, the Si content in the metal silicon raw materials is not less than 99%, and the raw materials in each batch need to be sampled and sent to the national refractory material quality supervision and inspection center for various detections after entering a factory, and the silicon nitride microcrystal plate is used after being qualified.
The production process of the silicon nitride microcrystal plate comprises the following steps:
s1, preparing coarse, medium and fine SiC particles containing more than 98% of SiC and industrial silicon powder containing more than 98% of Si, less than 10 microns and not more than 20 microns, batching to obtain a mixed material, obtaining a correct Si3N4-SiC brick raw material grading card from a technical responsible person during a batching stage by the batching person, weighing the raw materials one by one according to the items listed on the card, wherein the weighing error is not more than +/-0.2 Kg, placing the weighed raw materials in a mixing area, checking whether the grading and the weight of the raw materials meet the requirements by a technical person, and recording the batching time, the names of the batching person, the types of the raw materials and the like by the technical person.
S2, placing particles in raw materials into a mixer for mixing for 3 minutes, slowly pouring weighed water and water-soluble binding agent into the mixer for mixing for 5 minutes, wherein the mixing ratio of the water to the water-soluble binding agent is 2, so that the particles in the raw materials can fully absorb water, adding powdery raw materials and the binding agent after mixing for 5 minutes, mixing for 15 minutes, and finishing mixing, then pouring the mixed materials into a skip car for standing, performing secondary mixing after standing, drawing a mixing end to a forming workshop for forming, adopting dry-wet mixing during the mixing stage to help the raw material particles to fully absorb water, and after mixing is finished, judging the completion degree of mixing by checking whether too many blocky raw materials exist in the mixer, wherein the blocky raw materials are formally finished when the blocky raw materials are poured into the skip car for more than 168 hours, conveniently standing the mixed materials, drawing the formed mixed materials after standing, checking whether the water content of the raw materials is qualified, passing the mixed materials, pouring the mixed materials into the mixer for mixing again for 5 minutes (secondary mixing), then placing into the skip car, drawing the formed materials to the forming workshop for filling, and forming.
S3, pouring weighed raw materials into a mold, forming under the pressure of 19.6MPa, when a mixed material forming stage is carried out, firstly, weighing the weighed mixed raw materials correctly, then putting the weighed raw materials into the mold, carefully leveling to prevent the raw materials from leaking, starting the forming operation of the raw materials under the pressure of 19.6MPa and the pressure keeping time of 24 hours, checking whether the appearance and the size of each formed 20 bricks reach the standard by a forming operator, regarding a semi-finished product with +/-tolerance exceeding 1mm (including 1 mm) as a waste product, uniformly placing the waste product, crushing the waste product under the guidance of a technician, adding the waste product into a mixer for remixing in a small amount, wherein the density and the size of the semi-finished brick are checked by sampling at random by the technician in the forming process, whether cracks exist in the appearance and whether water content of water horns is defective, sealing the raw materials formed on the same day by plastic paper completely, preventing evaporation of the raw materials, detecting the water content of the raw materials when the next forming is required, and sending the raw materials to a mixing area when the water content is not up to the standard.
S4, placing the semi-finished product bricks into the porous metal drying plate, naturally drying the semi-finished product bricks in the shade, sending the semi-finished product bricks into a drying kiln for drying after the semi-finished product bricks are naturally dried in the shade, wherein the drying temperature in the drying kiln is 150-500 degrees, the heat preservation temperature is 180 degrees, during the drying stage, carefully placing the pressed semi-finished product bricks on the porous metal drying plate for naturally drying for more than 24 hours, placing the semi-finished product bricks after the drying in the shade into a drying vehicle and pushing the semi-finished product bricks into the drying kiln for drying, wherein the drying curve is divided into 3 stages, namely 80-degree heat preservation, 120-degree heat preservation and 180-degree heat preservation, and finally detecting the water content of the product by a technician after the drying is finished, the water content of the product after the drying must be less than 0.2 percent, and if the water content exceeds the standard, prolonging the heat preservation time of 180 degrees until the water content reaches the standard.
S5, placing the dried product into a kiln, adjusting the sintering control temperature, carrying out nitriding sintering treatment on the dried product, naturally cooling after sintering to obtain a finished product, wherein the sintering temperature of the sintering treatment is 800-1800 ℃, the heat preservation temperature is 800-1350 ℃, the product after sintering is naturally cooled to 200-210 ℃ below zero, the color of the product after nitriding sintering is offwhite and yellowish, the surface of the product does not show glass luster black, the color of the product after qualified nitriding sintering is offwhite and yellowish, the surface of the product does not show glass luster black, the product is qualified, placing the dried product into the kiln within 8 hours to prevent the product from absorbing moisture for too long time, randomly selecting 4 products for weighing and recording during kiln placing, placing the products into different positions of a kiln car, detecting after the products are taken out of the kiln, simultaneously loading the products into the kiln under the guidance of a technician, reserving gaps of about 2cm between the products so as to facilitate the transmission of nitrogen and heat, wherein the firing control is divided into 12 stages which account for about 120 hours, a heating curve is established according to the consumption of the nitrogen, a low-temperature long-time heat preservation system is implemented, heat preservation is carried out for a long time below 1350 ℃, so that the products reach the maximum nitriding rate, vacuumizing, nitrogen filling, nitrogen pressure and the like are taken charge of professional drivers in the firing process, the nitrogen required by nitriding is provided by a 100m & lt 3 & gt nitrogen making unit, two micro-oxygen analyzers and one dew point analyzer are used for detecting, the purity of the nitrogen is ensured to reach above 99.9995%, and finally, the products are naturally cooled to below 200 ℃ after the firing is finished, and the kiln car is pulled out of the bricks.
And finally, in the detection stage, firstly, observing that the surface of the product after nitriding and sintering is usually grey white and light yellow, if a large area of the product is black with glass luster, the phenomenon that oxygen permeates in the nitriding process is meant, the product of the batch is scrapped, and through 4 products marked in the fifth step, technicians are responsible for finding out 4 products marked during kiln loading, wiping and weighing the surfaces of the 4 products, comparing the weight of the 4 products before sintering, calculating the actual weight gain of the 4 products, and calculating the nitriding rate of the product, wherein the product can be considered to meet the national standard requirements in the case that the nitriding rate is more than or equal to 95 percent.
After the series of self-tests are qualified, workers are responsible for cleaning the surfaces of the products, boxing and packaging, the products with cracks, corner damages and obvious bending deformation in the treatment process are also treated as waste products, every 150-200 tons of Si3N4-SiC products are produced, 4-5 blocks are randomly extracted and sent to a related test center for testing, and various indexes of the products, such as normal-temperature compression resistance, normal-temperature bending resistance strength, high-temperature compression resistance, bending resistance strength, apparent porosity, heat conductivity coefficient, chemical analysis SiC and Si3N4 content, are tested to determine whether the products meet the national standards.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. The silicon nitride microcrystal plate is characterized in that: the composition of the silicon carbide powder is that coarse, medium and fine SiC particles containing SiC more than 98 percent and industrial silicon powder containing Si more than 98 percent, the particle size is less than 10 mu m, and the maximum particle size is not more than 20 mu m are taken as raw materials.
2. A process for producing a silicon nitride microcrystalline plate according to claim 1, characterized in that: the method comprises the following steps:
s1, preparing coarse, medium and fine SiC particles containing more than 98% of SiC and industrial silicon powder containing more than 98% of Si, less than 10 mu m and no more than 20 mu m at most, and mixing to obtain a mixed material;
s2, placing particles in the raw materials into a mixer for mixing for 3 minutes, slowly pouring weighed water and water-soluble binding agent into the mixer for mixing for 5 minutes according to a proportion so that the particles in the raw materials can fully absorb water, adding powdery raw materials and the binding agent after mixing for 5 minutes, mixing for 15 minutes to complete mixing, pouring the mixture into a skip car for standing, performing secondary mixing after standing, and pulling the mixed mixture to a forming workshop for forming;
s3, pouring the weighed raw materials into the mold, and simultaneously forming under the pressure of 19.6 MPa;
s4, placing the semi-finished bricks into the porous metal drying plate, naturally drying the semi-finished bricks in the shade, and conveying the semi-finished bricks into a drying kiln for drying after the semi-finished bricks are naturally dried in the shade;
and S5, placing the dried product into a kiln, adjusting the sintering control temperature, performing nitridation sintering treatment on the dried product, and naturally cooling after sintering to obtain a finished product.
3. The process for producing a silicon nitride microcrystalline plate according to claim 2, wherein: in the step two of S2, the mixing ratio of water to the water-soluble binding agent is 2.
4. The process for producing a silicon nitride microcrystalline plate according to claim 2, wherein: in the step S4, the drying treatment temperature in the drying kiln is 150-500 ℃, and the heat preservation temperature is 180 ℃.
5. The process for producing a silicon nitride microcrystalline plate according to claim 2, wherein: in the step S5, the firing temperature of the firing treatment is 800-1800 ℃, and the heat preservation temperature is 800-1350 ℃.
6. The process for producing a silicon nitride microcrystalline plate according to claim 2, wherein: and in the step S5, naturally cooling the product to 200-210 ℃ below zero after the product is fired.
7. The process for producing a silicon nitride microcrystalline plate according to claim 2, wherein: in the step S5, the color of the product after nitriding and sintering is grey white and light yellow, the surface of the product does not show black with glass luster, and the product is qualified.
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Citations (6)
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|---|---|---|---|---|
| GB726812A (en) * | 1952-11-11 | 1955-03-23 | Arthur Abbey | Improvements in or relating to silicon nitride materials |
| JP2002029850A (en) * | 2000-07-17 | 2002-01-29 | Denki Kagaku Kogyo Kk | Sintered silicon nitride compact and method for manufacturing the same |
| CN104003733A (en) * | 2014-05-19 | 2014-08-27 | 上海大学 | Preparation method of silicon nitride-combined silicon carbide fireproof material |
| CN105152663A (en) * | 2015-09-29 | 2015-12-16 | 北京科技大学 | Preparation method for silicon nitride and ferrosilicon nitride combined material |
| CN107311634A (en) * | 2017-07-19 | 2017-11-03 | 宜兴市锦泰耐火材料有限公司 | A kind of nitride bonded sandwich setter plate and preparation method thereof |
| CN107759238A (en) * | 2017-10-27 | 2018-03-06 | 中钢宁夏耐研滨河新材料有限公司 | The Nitride firing method of silicon nitride combined silicon carbide refractory product |
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- 2022-05-30 CN CN202210596507.2A patent/CN115368143A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB726812A (en) * | 1952-11-11 | 1955-03-23 | Arthur Abbey | Improvements in or relating to silicon nitride materials |
| JP2002029850A (en) * | 2000-07-17 | 2002-01-29 | Denki Kagaku Kogyo Kk | Sintered silicon nitride compact and method for manufacturing the same |
| CN104003733A (en) * | 2014-05-19 | 2014-08-27 | 上海大学 | Preparation method of silicon nitride-combined silicon carbide fireproof material |
| CN105152663A (en) * | 2015-09-29 | 2015-12-16 | 北京科技大学 | Preparation method for silicon nitride and ferrosilicon nitride combined material |
| CN107311634A (en) * | 2017-07-19 | 2017-11-03 | 宜兴市锦泰耐火材料有限公司 | A kind of nitride bonded sandwich setter plate and preparation method thereof |
| CN107759238A (en) * | 2017-10-27 | 2018-03-06 | 中钢宁夏耐研滨河新材料有限公司 | The Nitride firing method of silicon nitride combined silicon carbide refractory product |
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