CN113564711B - Method for rapidly growing high-quality silicon carbide - Google Patents
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Abstract
The invention relates to a method for rapidly growing high-quality silicon carbide, belonging to the technical field of silicon carbide crystal preparation. In order to solve the problem that the growth speed of the silicon carbide crystal prepared by the existing gas phase transmission method is reduced, the invention provides a method for quickly growing high-quality silicon carbide. The large-aperture porous silicon carbide raw material sheet can prevent silicon carbide gas from crystallizing on the surface of the raw material, and the growth speed of the silicon carbide crystal is improved by 20-30%; the porous silicon carbide raw material sheet with small aperture can filter carbon particles in gas components, and reduce the defects of inclusions, microtubes, dislocations and the like generated in the growth process of the silicon carbide crystal, thereby obtaining the silicon carbide crystal with higher quality.
Description
Technical Field
The invention belongs to the technical field of silicon carbide crystal preparation, and particularly relates to a method for rapidly growing high-quality silicon carbide.
Background
Silicon carbide is a stable compound of C and Si, and its lattice structure is composed of two sub-lattices arranged densely, with the C atoms surrounded by the periphery of each Si atom, or the Si atoms surrounded by the periphery of each C atom, bonded by oriented strong tetrahedral sp3 bonds. Because the silicon carbide has the characteristics of wide forbidden band, high thermal conductivity, high breakdown electric field, high radiation resistance and the like, the silicon carbide has wide application prospect in the aspects of high temperature, high frequency, high power, photoelectron, radiation resistance and the like.
In the process of producing silicon carbide crystals by the existing physical vapor transport method, silicon carbide powder is heated and sublimated into vapor phase, and the sublimated vapor phase is transported to seed crystals at the cold end and crystallized into blocky crystals under the protection of axial temperature gradient and inert atmosphere in a growth chamber. However, in the actual growth process, because the temperature at the edge of the crucible is higher, the silicon carbide raw material at the edge is sublimated and volatilized firstly, and the residual carbon is left at the original position after volatilization. The temperature at the center of the crucible is lower than the temperature at the edge of the crucible, and the raw material volatilized from the lower side is crystallized above the raw material having a lower temperature, preventing the gaseous raw material from moving toward the crystallization zone, resulting in a decrease in the growth rate of the crystal.
Disclosure of Invention
The invention provides a method for rapidly growing high-quality silicon carbide, aiming at solving the problem that the growth speed of the silicon carbide crystal prepared by the existing gas phase transmission method is reduced.
The technical scheme of the invention is as follows:
a method for rapidly growing high-quality silicon carbide comprises the following steps:
step one, preparing a porous silicon carbide raw material sheet:
organic foam pretreatment: cutting the polyurethane organic foam according to the size requirement of the porous silicon carbide raw material sheet, repeatedly washing the polyurethane organic foam with deionized water, sequentially soaking the polyurethane organic foam in an alkaline solution and a polyvinyl alcohol aqueous solution for pretreatment, and airing for later use; the polyurethane organic foam comprises two specifications of a pore size of 300-500 mu m and a pore size of 50-100 mu m;
(II) preparing slurry: sequentially adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution, uniformly stirring, and then carrying out ball milling to obtain slurry;
(III) preparing a blank body: adding the polyurethane organic foam prepared in the step (I) into the slurry obtained in the step (II), and repeatedly extruding to ensure that the slurry is fully immersed into pores of the polyurethane organic foam; placing the polyurethane organic foam fully soaked with the slurry between two glass plates, fully extruding to remove the redundant slurry to obtain a blank, and drying at room temperature for later use;
(IV) sintering: heating the green body obtained in the step (III) to 600 ℃ at a first heating rate, and then continuously heating to 2250 ℃ at a second heating rate for sintering to obtain large-aperture porous silicon carbide raw material sheets with the aperture of 300-500 mu m and small-aperture porous silicon carbide raw material sheets with the aperture of 50-100 mu m;
step two, preparing silicon carbide crystals:
laying conventional silicon carbide powder in a raw material area at the bottom of a crucible, laying a layer of small-aperture porous silicon carbide raw material sheet obtained in the first step on the silicon carbide powder, laying a layer of large-aperture porous silicon carbide raw material sheet obtained in the first step on the small-aperture porous silicon carbide raw material sheet, adhering silicon carbide seed crystals to the top of the crucible, vacuumizing the interior of the crucible, keeping the vacuum degree for 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, filling a mixed gas of nitrogen and argon into the interior of the crucible, filling 500torr, heating the interior of the crucible to 1800 ℃ while filling gas, starting to extract gas after heating to 1800 ℃, extracting gas to 10torr within 30min, keeping for 10h, extracting gas to 2torr within 10h, starting to grow the silicon carbide crystal, cooling after the crystal growth is finished, and filling argon to normal pressure to obtain the silicon carbide crystal.
Further, in the step one (I), the alkaline solution is 15-20 wt.% of sodium hydroxide solution, the alkaline solution is pretreated by soaking in a water bath at 40-50 ℃ for 3-5 h, and the obtained product is cleaned and dried; the soaking time for pretreatment in the polyvinyl alcohol aqueous solution is 20-30 h.
Further, the concentration of the polyvinyl alcohol aqueous solution in the step one (one) is 1 to 5 wt.%.
Further, the mass concentration of the silicon carbide powder in the slurry obtained in the first step (two) is 33-43 wt.%, the mass concentration of the carboxymethyl cellulose is 2-8 wt.%, and the mass concentration of the polyacrylamide is 1-3 wt.%.
Further, the ball milling time in the step one (second) is 4-6 h.
Further, in the first step (IV), the first heating rate is 2 ℃/min, the second heating rate is 5 ℃/min, and the sintering time is 2-3 h.
Further, in the step one (IV), the porosity of the large-aperture porous silicon carbide raw material sheet is 70-80%, and the thickness of the large-aperture porous silicon carbide raw material sheet is 1-6 mm; the porosity of the small-aperture porous silicon carbide raw material sheet is 50-60%, and the thickness of the small-aperture porous silicon carbide raw material sheet is 1-6 mm.
Further, the paving thickness of the conventional silicon carbide powder in the second step is 20-30 mm, the purity of the conventional silicon carbide powder is 99.9999%, and the particle size of the conventional silicon carbide powder is 50-300 microns.
Further, the vacuum degree of the vacuum pumping in the crucible in the step two is 10 -5 -10 -3 torr，
Furthermore, the volume ratio of the nitrogen to the argon in the mixed gas in the second step is 1: 9.
The invention has the beneficial effects that:
according to the invention, porous silicon carbide raw material pieces with different apertures and porosities are used as bases, raw materials are filled according to a lamellar shape, the upper layer of the porous silicon carbide raw material piece with the large aperture is used for preventing crystallization on the surface of the raw material with lower temperature in the process of silicon carbide gas rising from influencing the growth speed of crystals, the middle layer of the porous silicon carbide raw material piece with the small aperture is used for filtering carbon particles in gas components, the crystal quality is improved, and the situation that the raw materials are insufficient due to the fact that the apertures and the porosities of the porous silicon carbide are too large can be avoided by the lowest layer of compact silicon carbide powder.
The preparation method of the porous silicon carbide raw material sheet is simple, and different pore diameters and porosities are easy to control. The growth of the silicon carbide crystal by using the method provided by the invention can improve the growth speed of the silicon carbide crystal by 20-30%, and simultaneously can effectively eliminate the carbon particles formed after sublimation and volatilization of silicon carbide powder material from entering the silicon carbide crystal, thereby reducing the defects of inclusions, micro-tubes, dislocation and the like generated in the growth process of the silicon carbide crystal and obtaining the silicon carbide crystal with higher quality.
Drawings
FIG. 1 is a photograph showing the appearance of a high quality silicon carbide crystal produced in example 1 of the present invention;
FIG. 2 is a photograph of the appearance of the silicon carbide crystal prepared in comparative example 1.
Detailed Description
The technical solutions of the present invention are further described below with reference to the embodiments, but the present invention is not limited thereto, and any modifications or equivalent substitutions made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention should be covered in the protection scope of the present invention. The process equipment or apparatus not specifically mentioned in the following examples are conventional in the art, and if not specifically mentioned, the raw materials and the like used in the examples of the present invention are commercially available; unless otherwise specified, all technical means used in the examples of the present invention are conventional means well known to those skilled in the art.
Example 1
The embodiment provides a method for rapidly growing high-quality silicon carbide, which comprises the following steps:
step one, preparing a porous silicon carbide raw material sheet:
organic foam pretreatment:
preparing polyurethane organic foam with two specifications of 300-500 mu m of pore diameter, 70-80% of porosity, 50-100 mu m of pore diameter and 50-60% of porosity.
Cutting polyurethane organic foam according to the size requirement of a porous silicon carbide raw material sheet, repeatedly washing with deionized water, soaking the washed polyurethane organic foam sheet in 15 wt.% of sodium hydroxide solution for 3 hours under the condition of water bath at 40 ℃, cleaning and airing; dissolving polyvinyl alcohol in deionized water at 90 ℃ in a water bath condition to obtain a 2 wt.% polyvinyl alcohol aqueous solution, soaking the polyurethane organic foam sheet treated by sodium hydroxide in the polyvinyl alcohol aqueous solution for 24 hours, and airing for later use;
(II) preparing slurry:
adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution in sequence, uniformly stirring, and then carrying out ball milling for 4 hours to obtain slurry, wherein the mass concentration of the silicon carbide powder in the slurry is 38 wt.%, the mass concentration of the carboxymethyl cellulose is 5 wt.%, and the mass concentration of the polyacrylamide is 2 wt.%.
The slurry is prepared from conventional silicon carbide powder with the purity of 99.9999% and the particle size of 50-300 mu m.
(III) preparing a blank body:
introducing the slurry uniformly mixed in the step (II) into an open container, putting the polyurethane organic foam prepared in the step (I) into the slurry obtained in the step (II), and repeatedly extruding to ensure that the slurry is fully immersed into pores of the polyurethane organic foam sheet; preparing two glass plates, placing the polyurethane organic foam sheet fully soaked with the slurry between the two glass plates, fully extruding to remove redundant slurry to obtain a blank, and drying at room temperature for later use;
(IV) sintering:
heating the blank obtained in the step (III) to 600 ℃ at the heating rate of 2 ℃/min, then continuously heating to 2250 ℃ at the heating rate of 5 ℃/min, and sintering for 2h to obtain a large-aperture porous silicon carbide raw material sheet with the aperture of 300-500 mu m, the porosity of 70-80% and the thickness of 3mm and a small-aperture porous silicon carbide raw material sheet with the aperture of 50-100 mu m, the porosity of 50-60% and the thickness of 3 mm;
step two, preparing silicon carbide crystals:
lay the conventional carborundum powder that thickness is 20mm in crucible bottom raw materials district, the purity of conventional carborundum powder is 99.9999%, and the particle diameter is 50 ~ 300 mu m, lays the one-layer thickness and is 3 mm's step one and obtains small aperture porous carborundum raw materials piece on carborundum powder lay the one-layer thickness and be 3 mm's step one and obtain large aperture porous carborundum raw materials piece on the small aperture porous carborundum raw materials piece, paste the carborundum seed crystal in the crucible top, the inside evacuation of crucible is to and 10 -5 -10 -3 torr, keeping the vacuum degree within 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, then filling mixed gas of nitrogen and argon with the volume ratio of 1:9 into the crucible, filling the mixed gas to 500torr, heating the interior of the crucible to 1800 ℃ within 3h while filling gas, starting to extract gas after the temperature is raised to 1800 ℃, extracting gas to 10torr within 30min, keeping the temperature for 10h, then extracting gas to 2torr within 10h, starting to grow the silicon carbide crystal, keeping the crystal growth time to 96h, cooling after the crystal growth is finished, filling argon to normal pressure, and obtaining the silicon carbide crystal with the crystal growth height of 20 mm.
In the embodiment, polyurethane organic foams with different pore diameters and porosities are selected as the base material, the base material is added into silicon carbide slurry to prepare the blank, and then the organic foams, the carboxymethyl cellulose serving as the adhesive, the polyacrylamide serving as the dispersing agent and the polyvinyl alcohol in the blank are removed by sintering, so that porous silicon carbide raw material pieces with the pore diameters and porosities close to those of the polyurethane organic foams are left.
Based on the porous silicon carbide raw material pieces with different apertures and porosities, the raw material is filled according to the lamellar shape, the upper-layer large-aperture porous silicon carbide raw material piece can prevent the crystal growth speed from being influenced by crystallization on the surface of the raw material with lower temperature in the process of silicon carbide gas rising, and the growth speed of the silicon carbide crystal can be improved by 20-30%. The porous silicon carbide raw material sheet with the small aperture in the middle layer is used for filtering carbon particles formed after silicon carbide powder in the gas component is sublimated and volatilized, so that the defects of inclusions, microtubes, dislocations and the like generated when the carbon particles enter the silicon carbide crystal are eliminated, and the crystal quality is improved; the situation that the porous silicon carbide is insufficient in raw materials due to overlarge pore diameter and porosity can be avoided by the aid of the compact silicon carbide powder at the lowermost layer, and accordingly silicon carbide crystals with higher quality are obtained.
FIG. 1 is a photograph showing the appearance of the silicon carbide crystal produced in this example, from which it can be seen that the surface of the silicon carbide crystal was smooth and free of defects, and had high crystal quality.
Example 2
The embodiment provides a method for rapidly growing high-quality silicon carbide, which comprises the following steps:
step one, preparing a porous silicon carbide raw material sheet:
organic foam pretreatment:
preparing polyurethane organic foam with two specifications of 300-500 mu m of pore diameter, 70-80% of porosity, 50-100 mu m of pore diameter and 50-60% of porosity.
Cutting polyurethane organic foam according to the size requirement of a porous silicon carbide raw material sheet, repeatedly washing with deionized water, soaking the washed polyurethane organic foam sheet in 15 wt.% of sodium hydroxide solution, soaking for 5 hours in a water bath at 42 ℃, cleaning, and airing; dissolving polyvinyl alcohol in deionized water at 90 ℃ in a water bath condition to obtain 1 wt.% of polyvinyl alcohol aqueous solution, soaking the polyurethane organic foam sheet treated by sodium hydroxide in the polyvinyl alcohol aqueous solution for 20 hours, and airing for later use;
(II) preparing slurry:
adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution in sequence, uniformly stirring, and carrying out ball milling for 4 hours to obtain slurry, wherein the mass concentration of the silicon carbide powder in the slurry is 33 wt.%, the mass concentration of the carboxymethyl cellulose is 8 wt.%, and the mass concentration of the polyacrylamide is 3 wt.%.
The slurry is prepared from conventional silicon carbide powder with the purity of 99.9999% and the particle size of 50-300 mu m.
(III) preparing a blank body:
introducing the slurry uniformly mixed in the step (II) into an open container, putting the polyurethane organic foam prepared in the step (I) into the slurry obtained in the step (II), and repeatedly extruding to ensure that the slurry is fully immersed into pores of the polyurethane organic foam sheet; preparing two glass plates, placing the polyurethane organic foam sheet fully soaked with the slurry between the two glass plates, fully extruding to remove the redundant slurry to obtain a blank, and drying at room temperature for later use;
(IV) sintering:
heating the green body obtained in the step (III) to 600 ℃ at the heating rate of 2 ℃/min, and preventing the polyurethane organic foam from volatilizing too fast due to too fast heating rate to cause the collapse of the green body; continuously heating to 2250 ℃ at the heating rate of 5 ℃/min, sintering for 2h, and cooling along with the furnace to obtain large-aperture porous silicon carbide raw material sheets with the aperture of 300-500 mu m, the porosity of 70-80 percent and the thickness of 3mm and small-aperture porous silicon carbide raw material sheets with the aperture of 50-100 mu m, the porosity of 50-60 percent and the thickness of 5 mm;
step two, preparing silicon carbide crystals:
lay the conventional carborundum powder that thickness is 20mm in crucible bottom raw materials district, the purity of conventional carborundum powder is 99.9999%, and the particle diameter is 50 ~ 300 mu m, lays the one-layer thickness and is step one gained small aperture porous carborundum raw materials piece of 5mm on carborundum powder lay the one-layer thickness and be step one gained large aperture porous carborundum raw materials piece of 3mm on the small aperture porous carborundum raw materials piece, paste the carborundum seed crystal in the crucible top, the inside evacuation of crucible is to and 10 -5 -10 -3 torr, keeping the vacuum degree within 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, then filling the mixed gas of nitrogen and argon with the volume ratio of 1:9 into the crucible, filling the mixture to 500torr, and filling the mixtureHeating the internal temperature of the crucible to 1800 ℃ within 3h, raising the temperature to 1800 ℃, then starting to exhaust, exhausting to 10torr within 30min, keeping for 10h, then exhausting to 2torr within 10h, starting to grow the silicon carbide crystal, wherein the crystal growth time is 100h, cooling after the crystal growth is finished, and filling argon to normal pressure to obtain the silicon carbide crystal with the crystal growth height of 18 mm.
Example 3
The embodiment provides a method for rapidly growing high-quality silicon carbide, which comprises the following steps:
step one, preparing a porous silicon carbide raw material sheet:
organic foam pretreatment:
preparing polyurethane organic foam with two specifications of 300-500 mu m of pore diameter, 70-80% of porosity, 50-100 mu m of pore diameter and 50-60% of porosity.
Cutting polyurethane organic foam according to the size requirement of a porous silicon carbide raw material sheet, repeatedly washing with deionized water, soaking the washed polyurethane organic foam sheet in 18 wt.% of sodium hydroxide solution, soaking for 4 hours in a water bath at 45 ℃, cleaning, and airing; dissolving polyvinyl alcohol in deionized water under the condition of water bath at 90 ℃ to obtain 3 wt.% of polyvinyl alcohol aqueous solution, soaking the polyurethane organic foam sheet treated by sodium hydroxide in the polyvinyl alcohol aqueous solution for 22 hours, and airing for later use;
(II) preparing slurry:
adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution in sequence, uniformly stirring, and carrying out ball milling for 5 hours to obtain slurry, wherein the mass concentration of the silicon carbide powder in the slurry is 35 wt.%, the mass concentration of the carboxymethyl cellulose is 7 wt.%, and the mass concentration of the polyacrylamide is 3 wt.%.
The slurry is prepared from conventional silicon carbide powder with the purity of 99.9999% and the particle size of 50-300 mu m.
(III) preparing a blank body:
introducing the slurry uniformly mixed in the step (II) into an open container, putting the polyurethane organic foam prepared in the step (I) into the slurry obtained in the step (II), and repeatedly extruding to ensure that the slurry is fully immersed into pores of the polyurethane organic foam sheet; preparing two glass plates, placing the polyurethane organic foam sheet fully soaked with the slurry between the two glass plates, fully extruding to remove the redundant slurry to obtain a blank, and drying at room temperature for later use;
(IV) sintering:
heating the blank obtained in the step (III) to 600 ℃ at the heating rate of 2 ℃/min, then continuously heating to 2250 ℃ at the heating rate of 5 ℃/min, and sintering for 2h to obtain a large-aperture porous silicon carbide raw material sheet with the aperture of 300-500 mu m, the porosity of 70-80% and the thickness of 4mm and a small-aperture porous silicon carbide raw material sheet with the aperture of 50-100 mu m, the porosity of 50-60% and the thickness of 2 mm;
step two, preparing silicon carbide crystals:
lay the conventional carborundum powder that thickness is 25mm in crucible bottom raw materials district, the purity of conventional carborundum powder is 99.9999%, and the particle diameter is 50 ~ 300 mu m, lays the one-layer thickness and is 2 mm's step one and obtains small aperture porous carborundum raw materials piece on carborundum powder lay the one-layer thickness and be 4 mm's step one and obtain large aperture porous carborundum raw materials piece on the small aperture porous carborundum raw materials piece, paste the carborundum seed crystal in the crucible top, the inside evacuation of crucible is to and 10 -5 -10 -3 And (2) torr, keeping the vacuum degree within 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, then filling mixed gas of nitrogen and argon with the volume ratio of 1:9 into the crucible, filling the mixed gas to 500torr, heating the interior of the crucible to 1800 ℃ within 3h while filling the mixed gas, heating the interior of the crucible to 1800 ℃, starting pumping after the temperature is raised to 1800 ℃, pumping to 10torr within 30min, keeping the temperature for 10h, then pumping to 2torr within 10h, starting the growth of the silicon carbide crystal, keeping the crystal growth time for 100h, cooling after the crystal growth is finished, and filling argon to normal pressure to obtain the silicon carbide crystal with the crystal growth height of 18 mm.
Example 4
The embodiment provides a method for rapidly growing high-quality silicon carbide, which comprises the following steps:
step one, preparing a porous silicon carbide raw material sheet:
organic foam pretreatment:
preparing polyurethane organic foam with two specifications of 300-500 mu m of pore diameter, 70-80% of porosity, 50-100 mu m of pore diameter and 50-60% of porosity.
Cutting polyurethane organic foam according to the size requirement of a porous silicon carbide raw material sheet, repeatedly washing with deionized water, soaking the washed polyurethane organic foam sheet in 18 wt.% sodium hydroxide solution, soaking for 4 hours in a water bath at 48 ℃, cleaning, and airing; dissolving polyvinyl alcohol in deionized water under the condition of water bath at 90 ℃ to obtain 4 wt.% of polyvinyl alcohol aqueous solution, soaking the polyurethane organic foam sheet treated by sodium hydroxide in the polyvinyl alcohol aqueous solution for 25 hours, and airing for later use;
(II) preparing slurry:
adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution in sequence, uniformly stirring, and then carrying out ball milling for 5 hours to obtain slurry, wherein the mass concentration of the silicon carbide powder in the slurry is 40 wt.%, the mass concentration of the carboxymethyl cellulose is 4 wt.%, and the mass concentration of the polyacrylamide is 1 wt.%.
The slurry is prepared from conventional silicon carbide powder with the purity of 99.9999% and the particle size of 50-300 mu m.
(III) preparing a blank body:
introducing the slurry uniformly mixed in the step (II) into an open container, putting the polyurethane organic foam prepared in the step (I) into the slurry obtained in the step (II), and repeatedly extruding to ensure that the slurry is fully immersed into pores of the polyurethane organic foam sheet; preparing two glass plates, placing the polyurethane organic foam sheet fully soaked with the slurry between the two glass plates, fully extruding to remove redundant slurry to obtain a blank, and drying at room temperature for later use;
(IV) sintering:
heating the blank obtained in the step (III) to 600 ℃ at the heating rate of 2 ℃/min, then continuously heating to 2250 ℃ at the heating rate of 5 ℃/min, and sintering for 3h to obtain large-aperture porous silicon carbide raw material sheets with the aperture of 300-500 mu m, the porosity of 70-80% and the thickness of 2mm and small-aperture porous silicon carbide raw material sheets with the aperture of 50-100 mu m, the porosity of 50-60% and the thickness of 2 mm;
step two, preparing silicon carbide crystals:
lay the conventional carborundum powder that thickness is 25mm in crucible bottom raw materials district, the purity of conventional carborundum powder is 99.9999%, and the particle diameter is 50 ~ 300 mu m, lays the one-layer thickness and is 2 mm's step one and obtains small aperture porous carborundum raw materials piece on carborundum powder lay the one-layer thickness and be 2 mm's step one and obtain large aperture porous carborundum raw materials piece on the small aperture porous carborundum raw materials piece, paste the carborundum seed crystal in the crucible top, the inside evacuation of crucible is to and 10 -5 -10 -3 torr, keeping the vacuum degree within 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, then filling mixed gas of nitrogen and argon with the volume ratio of 1:9 into the crucible, filling the mixed gas to 500torr, heating the interior of the crucible to 1800 ℃ within 3h while filling gas, starting to extract gas after the temperature is raised to 1800 ℃, extracting gas to 10torr within 30min, keeping the temperature for 10h, then extracting gas to 2torr within 10h, starting to grow the silicon carbide crystal, keeping the crystal growth time to 98h, cooling after the crystal growth is finished, filling argon to normal pressure, and obtaining the silicon carbide crystal with the crystal growth height of 20 mm.
Example 5
The embodiment provides a method for rapidly growing high-quality silicon carbide, which comprises the following steps:
step one, preparing a porous silicon carbide raw material sheet:
organic foam pretreatment:
preparing polyurethane organic foam with two specifications of 300-500 mu m of pore diameter, 70-80% of porosity, 50-100 mu m of pore diameter and 50-60% of porosity.
Cutting polyurethane organic foam according to the size requirement of a porous silicon carbide raw material sheet, repeatedly washing with deionized water, soaking the washed polyurethane organic foam sheet in 20 wt.% sodium hydroxide solution, soaking for 3 hours in a water bath at 50 ℃, cleaning, and airing; dissolving polyvinyl alcohol in deionized water under the condition of water bath at 90 ℃ to obtain 2 wt.% of polyvinyl alcohol aqueous solution, soaking the polyurethane organic foam sheet treated by sodium hydroxide in the polyvinyl alcohol aqueous solution for 28 hours, and airing for later use;
(II) preparing slurry:
adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution in sequence, uniformly stirring, and then carrying out ball milling for 6 hours to obtain slurry, wherein the mass concentration of the silicon carbide powder in the slurry is 38 wt.%, the mass concentration of the carboxymethyl cellulose is 6 wt.%, and the mass concentration of the polyacrylamide is 1 wt.%.
The slurry is prepared from conventional silicon carbide powder with the purity of 99.9999% and the particle size of 50-300 mu m.
(III) preparing a blank body:
introducing the slurry uniformly mixed in the step (II) into an open container, putting the polyurethane organic foam prepared in the step (I) into the slurry obtained in the step (II), and repeatedly extruding to ensure that the slurry is fully immersed into pores of the polyurethane organic foam sheet; preparing two glass plates, placing the polyurethane organic foam sheet fully soaked with the slurry between the two glass plates, fully extruding to remove redundant slurry to obtain a blank, and drying at room temperature for later use;
(IV) sintering:
heating the blank obtained in the step (three) to 600 ℃ at the heating rate of 2 ℃/min, then continuously heating to 2250 ℃ at the heating rate of 5 ℃/min, and sintering for 3 hours to obtain large-aperture porous silicon carbide raw material sheets with the aperture of 300-500 mu m, the porosity of 70-80% and the thickness of 3mm and small-aperture porous silicon carbide raw material sheets with the aperture of 50-100 mu m, the porosity of 50-60% and the thickness of 2 mm;
step two, preparing silicon carbide crystals:
lay the conventional carborundum powder that thickness is 30mm in crucible bottom raw materials district, the purity of conventional carborundum powder is 99.9999%, and the particle diameter is 50 ~ 300 mu m, lays the one-layer thickness and is 2 mm's step one and obtains small aperture porous carborundum raw materials piece on carborundum powder lay the one-layer thickness and be 3 mm's step one and obtain large aperture porous carborundum raw materials piece on the small aperture porous carborundum raw materials piece, paste the carborundum seed crystal in the crucible top, the inside evacuation of crucible is to and 10 -5 -10 -3 torr, keeping the vacuum degree within 1.5h, heating the interior of the crucible to 1300 ℃, and keeping the temperature for 0.5hAnd filling a mixed gas of nitrogen and argon in a volume ratio of 1:9 into the crucible, filling the mixed gas to 500torr, heating the temperature in the crucible to 1800 ℃ within 3h while filling the mixed gas, starting pumping after the temperature is raised to 1800 ℃, pumping to 10torr within 30min, keeping for 10h, pumping to 2torr within 10h, starting the growth of the silicon carbide crystal, wherein the crystal growth time is 103h, cooling after the crystal growth is finished, and filling argon to normal pressure to obtain the silicon carbide crystal with the crystal growth height of 20 mm.
Example 6
The embodiment provides a method for rapidly growing high-quality silicon carbide, which comprises the following steps:
step one, preparing a porous silicon carbide raw material sheet:
organic foam pretreatment:
preparing polyurethane organic foam with two specifications of 300-500 mu m of pore diameter, 70-80% of porosity, 50-100 mu m of pore diameter and 50-60% of porosity.
Cutting polyurethane organic foam according to the size requirement of a porous silicon carbide raw material sheet, repeatedly washing with deionized water, soaking the washed polyurethane organic foam sheet in 20 wt.% of sodium hydroxide solution, soaking for 3h under the water bath condition of 50 ℃, cleaning, and airing; dissolving polyvinyl alcohol in deionized water under the condition of water bath at 90 ℃ to obtain 5 wt.% of polyvinyl alcohol aqueous solution, soaking the polyurethane organic foam sheet treated by sodium hydroxide in the polyvinyl alcohol aqueous solution for 30 hours, and airing for later use;
(II) preparing slurry:
adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution in sequence, uniformly stirring, and then carrying out ball milling for 6 hours to obtain slurry, wherein the mass concentration of the silicon carbide powder in the obtained slurry is 43 wt.%, the mass concentration of the carboxymethyl cellulose is 2 wt.%, and the mass concentration of the polyacrylamide is 1 wt.%.
The slurry is prepared from conventional silicon carbide powder with the purity of 99.9999% and the particle size of 50-300 mu m.
(III) preparing a blank body:
introducing the slurry uniformly mixed in the step (II) into an open container, putting the polyurethane organic foam prepared in the step (I) into the slurry obtained in the step (II), and repeatedly extruding to ensure that the slurry is fully immersed into pores of the polyurethane organic foam sheet; preparing two glass plates, placing the polyurethane organic foam sheet fully soaked with the slurry between the two glass plates, fully extruding to remove redundant slurry to obtain a blank, and drying at room temperature for later use;
(IV) sintering:
heating the blank obtained in the step (three) to 600 ℃ at the heating rate of 2 ℃/min, then continuously heating to 2250 ℃ at the heating rate of 5 ℃/min, and sintering for 3 hours to obtain large-aperture porous silicon carbide raw material sheets with the aperture of 300-500 mu m, the porosity of 70-80% and the thickness of 3mm and small-aperture porous silicon carbide raw material sheets with the aperture of 50-100 mu m, the porosity of 50-60% and the thickness of 5 mm;
step two, preparing silicon carbide crystals:
lay the conventional carborundum powder that thickness is 30mm in crucible bottom raw materials district, the purity of conventional carborundum powder is 99.9999%, and the particle diameter is 50 ~ 300 mu m, lays the one-layer thickness and is step one gained small aperture porous carborundum raw materials piece of 5mm on carborundum powder lay the one-layer thickness and be step one gained large aperture porous carborundum raw materials piece of 3mm on the small aperture porous carborundum raw materials piece, paste the carborundum seed crystal in the crucible top, the inside evacuation of crucible is to and 10 -5 -10 -3 And (2) torr, keeping the vacuum degree within 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, then filling mixed gas of nitrogen and argon with the volume ratio of 1:9 into the crucible, filling the mixed gas to 500torr, heating the interior of the crucible to 1800 ℃ within 3h while filling gas, starting pumping after the temperature is raised to 1800 ℃, pumping to 10torr within 30min, keeping the temperature for 10h, then pumping to 2torr within 10h, starting the growth of the silicon carbide crystal, keeping the crystal growth time for 100h, cooling after the crystal growth is finished, and filling argon to normal pressure to obtain the silicon carbide crystal with the crystal growth height of 19 mm.
Comparative example 1
In the comparative example, the conventional silicon carbide powder is used as the raw material to prepare the silicon carbide crystal, and the conventional silicon carbide powder with the thickness of 50 is paved in the raw material area at the bottom of the crucibleThe purity of the silicon carbide seed crystal is 99.9999%, the particle size of the silicon carbide seed crystal is 50-300 mu m, the silicon carbide seed crystal is adhered to the top of a crucible, and the interior of the crucible is vacuumized to 10 DEG -5 -10 -3 And (2) torr, keeping the vacuum degree within 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, then filling mixed gas of nitrogen and argon with the volume ratio of 1:9 into the crucible, filling the mixed gas to 500torr, heating the interior of the crucible to 1800 ℃ within 3h while filling the mixed gas, heating the interior of the crucible to 1800 ℃, starting pumping after the temperature is raised to 1800 ℃, pumping to 10torr within 30min, keeping the temperature for 10h, then pumping to 2torr within 10h, starting the growth of the silicon carbide crystal, keeping the crystal growth time for 120h, cooling after the crystal growth is finished, and filling argon to normal pressure to obtain the silicon carbide crystal with the crystal growth height of 20 mm.
FIG. 2 is a photograph showing the appearance of the silicon carbide crystal prepared in this comparative example, from which it can be seen that the surface of the silicon carbide crystal had defects visible to the naked eye.
Comparing the crystal growth times of example 1 and comparative example 1, it can be seen that the crystal growth rate of example 1 is significantly higher than that of comparative example 1, and the silicon carbide crystal with the same growth height is grown, and the method provided in example 1 can reduce the crystal growth time by 20%. This demonstrates that the silicon carbide crystal growth method provided by the present invention provides a higher quality silicon carbide crystal in a shorter time.
Claims (10)
1. A method for rapidly growing high-quality silicon carbide is characterized by comprising the following steps:
step one, preparing a porous silicon carbide raw material sheet:
step 1.1 organic foam pretreatment: cutting polyurethane organic foam according to the size requirement of a porous silicon carbide raw material sheet, repeatedly washing the polyurethane organic foam with deionized water, sequentially soaking the polyurethane organic foam in an alkaline solution and a polyvinyl alcohol aqueous solution for pretreatment, and airing for later use; the polyurethane organic foam comprises two specifications of a pore size of 300-500 mu m and a pore size of 50-100 mu m;
step 1.2 preparation of slurry: sequentially adding silicon carbide powder and polyacrylamide into a carboxymethyl cellulose aqueous solution, uniformly stirring, and then carrying out ball milling to obtain slurry;
step 1.3, preparing a blank: adding the polyurethane organic foam prepared in the step 1.1 into the slurry obtained in the step 1.2, and repeatedly extruding to ensure that the slurry is fully immersed in pores of the polyurethane organic foam; placing the polyurethane organic foam fully soaked with the slurry between two glass plates, fully extruding to remove redundant slurry to obtain a blank, and drying at room temperature for later use;
step 1.4, sintering: heating the blank obtained in the step 1.3 to 600 ℃ at a first heating rate, and then continuously heating to 2250 ℃ at a second heating rate for sintering to obtain a large-aperture porous silicon carbide raw material sheet with the aperture of 300-500 mu m and a small-aperture porous silicon carbide raw material sheet with the aperture of 50-100 mu m;
step two, preparing silicon carbide crystals:
laying conventional silicon carbide powder in a raw material area at the bottom of a crucible, laying a layer of small-aperture porous silicon carbide raw material sheet obtained in the first step on the silicon carbide powder, laying a layer of large-aperture porous silicon carbide raw material sheet obtained in the first step on the small-aperture porous silicon carbide raw material sheet, adhering silicon carbide seed crystals to the top of the crucible, vacuumizing the interior of the crucible, keeping the vacuum degree for 1.5h, heating the interior of the crucible to 1300 ℃, keeping the temperature for 0.5h, filling a mixed gas of nitrogen and argon into the interior of the crucible, filling 500torr, heating the interior of the crucible to 1800 ℃ while filling gas, starting to extract gas after heating to 1800 ℃, extracting gas to 10torr within 30min, keeping for 10h, extracting gas to 2torr within 10h, starting to grow the silicon carbide crystal, cooling after the crystal growth is finished, and filling argon to normal pressure to obtain the silicon carbide crystal.
2. The method for rapidly growing high-quality silicon carbide according to claim 1, wherein in the step 1.1, the alkaline solution is 15-20 wt.% sodium hydroxide solution, the alkaline solution is pretreated by soaking in a water bath at 40-50 ℃ for 3-5 h, and the silicon carbide is cleaned and dried; the soaking time for pretreatment in the polyvinyl alcohol aqueous solution is 20-30 h.
3. The method for rapidly growing high quality silicon carbide according to claim 1 or 2 wherein the concentration of the aqueous solution of polyvinyl alcohol in step 1.1 is 1 to 5 wt.%.
4. The method for rapidly growing high-quality silicon carbide according to claim 3, wherein the mass concentration of the silicon carbide powder in the slurry obtained in step 1.2 is 33-43 wt.%, the mass concentration of the carboxymethyl cellulose is 2-8 wt.%, and the mass concentration of the polyacrylamide is 1-3 wt.%.
5. The method for rapidly growing high quality silicon carbide according to claim 4 wherein the ball milling time in step 1.2 is 4-6 hours.
6. The method according to claim 5, wherein the first temperature-raising rate in step 1.4 is 2 ℃/min, the second temperature-raising rate is 5 ℃/min, and the sintering time is 2to 3 hours.
7. The method for rapidly growing high-quality silicon carbide according to claim 6, wherein the porosity of the large-aperture porous silicon carbide raw material sheet in the step 1.4 is 70-80% and the thickness is 1-6 mm; the porosity of the small-aperture porous silicon carbide raw material sheet is 50-60%, and the thickness of the small-aperture porous silicon carbide raw material sheet is 1-6 mm.
8. The method for rapidly growing high-quality silicon carbide according to claim 7, wherein the conventional silicon carbide powder material in the second step is laid to have a thickness of 20 to 30mm, and has a purity of 99.9999% and a particle size of 50 to 300 μm.
9. The method for rapidly growing high-quality silicon carbide according to claim 8, wherein the degree of vacuum applied to the inside of the crucible in the second step is 10 -5 -10 -3 torr。
10. The method of claim 9, wherein the volume ratio of nitrogen to argon in the mixture gas in step two is 1: 9.
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