CN119082862A - Polycrystalline silicon carbide rod, preparation device and method thereof, and polycrystalline silicon carbide powder - Google Patents
Polycrystalline silicon carbide rod, preparation device and method thereof, and polycrystalline silicon carbide powder Download PDFInfo
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- CN119082862A CN119082862A CN202411578767.2A CN202411578767A CN119082862A CN 119082862 A CN119082862 A CN 119082862A CN 202411578767 A CN202411578767 A CN 202411578767A CN 119082862 A CN119082862 A CN 119082862A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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Abstract
The invention belongs to the technical field of silicon carbide crystals, and particularly relates to a polycrystalline silicon carbide rod, a preparation device and a preparation method thereof and polycrystalline silicon carbide powder. The preparation device comprises a reactor, wherein the reactor comprises a bottom plate, a cover body and a deposition carrier in the cover body, a suction hole is formed in the center of the bottom plate, an electrode connected with the deposition carrier is arranged outside the suction hole in a penetrating mode, an air inlet hole is formed in the outer side of the electrode, an air inlet pipe extending to the inside of the reactor through the air inlet hole, a negative pressure component comprising an air exhaust pipe, an air exhaust part, an air exhaust control part and a negative pressure monitoring part is arranged, a first end of the air exhaust pipe is communicated with the inside of the reactor through the suction hole, the end portion of the first end of the air exhaust pipe is lower than the lower end of the deposition carrier, a second end of the air exhaust pipe is communicated with the air exhaust part, the negative pressure monitoring part monitors whether the pressure in the reactor is in a range of 0.001bar-0.1 bar, and the air exhaust control part is respectively connected with the negative pressure monitoring part and the air exhaust part, and the compactness of a silicon carbide rod and the purity of powder can be improved.
Description
Technical Field
The invention belongs to the technical field of silicon carbide crystals, and particularly relates to a polycrystalline silicon carbide rod, a preparation device and a preparation method thereof and polycrystalline silicon carbide powder.
Background
The silicon carbide single crystal substrate material belongs to a wide forbidden band semiconductor material, has the advantages of high pressure resistance, high temperature resistance, high frequency, low loss and the like, and has been widely applied to the fields of high-power electronic devices, microwave radio frequency devices and the like.
The current industrialized preparation method of the silicon carbide single crystal material mainly comprises a physical vapor transport method (PVT), namely, a polycrystalline silicon carbide powder raw material is arranged in a closed cavity formed by a graphite crucible and a crucible cover, a silicon carbide seed crystal sheet is adhered to the inner wall of the crucible cover, the polycrystalline silicon carbide powder raw material at the lower part of the graphite crucible is sublimated by heating in an inert atmosphere environment, and the sublimated gas grows and crystallizes on the silicon carbide seed crystal to obtain the silicon carbide single crystal.
In order to obtain the polycrystalline silicon carbide powder raw material, the polycrystalline silicon carbide rod can be obtained by chemical vapor deposition of silicon source gas and carbon source gas on a carrier, and the polycrystalline silicon carbide rod is obtained after being crushed, however, the prepared polycrystalline silicon carbide rod is easy to have more hole structures, the hole structures are easy to absorb materials such as the silicon source gas, the carbon source gas, carrier gas and the like, and are easy to absorb dust and gas suspended in air, the purity of the polycrystalline silicon carbide powder is influenced after crushing, and the polycrystalline silicon carbide powder is further used for growing silicon carbide single crystal materials, and the quality of silicon carbide single crystals is influenced.
It should be noted that this section of the disclosure only provides a background related to the present disclosure, and does not necessarily constitute prior art or known technology.
Disclosure of Invention
The invention aims to overcome the defect that a plurality of hole structures are easy to exist on a polycrystalline silicon carbide rod prepared by chemical vapor deposition reaction in the prior art, impurities are easy to adsorb in the hole structures, and the purity of polycrystalline silicon carbide powder is influenced.
In order to achieve the above object, in a first aspect, the present invention provides a preparation apparatus for a high-density polycrystalline silicon carbide rod, comprising:
The reactor comprises a bottom plate, a cover body covered on the bottom plate and a vertical deposition carrier positioned in the cover body, wherein a suction hole is formed in the center of the bottom plate, a vertical electrode penetrates through the bottom plate, the electrode is positioned outside the suction hole, the upper end of the electrode is connected with the lower end of the deposition carrier, and an air inlet hole is formed in the outer side of the electrode on the bottom plate;
one end of the air inlet pipe extends to the inside of the reactor through the air inlet hole, and a nozzle is arranged on a pipe section of the air inlet pipe positioned in the reactor;
The negative pressure assembly comprises an exhaust pipe, an exhaust part, an exhaust control part and a negative pressure monitoring part, wherein the first end of the exhaust pipe is communicated with the inside of the reactor through an exhaust hole, the end part of the first end of the exhaust pipe is lower than the lower end of the deposition carrier, the second end of the exhaust pipe is communicated with the exhaust part, the negative pressure monitoring part monitors whether the pressure in the reactor is in the range of 0.001bar-0.1 bar or not, the exhaust control part is respectively connected with the negative pressure monitoring part and the exhaust part, one end of the air inlet pipe extends to the upper part of the deposition carrier through an air inlet hole, a plurality of nozzles are arranged on the side part, close to the deposition carrier, of the pipe section of the air inlet pipe, the nozzles are arranged at intervals along the axial direction of the air inlet pipe, the uppermost nozzle is positioned on the deposition carrier, and the nozzle at the lowermost end is positioned on the first end of the pipe and is at a vertical distance of more than 50cm from the first end of the exhaust pipe.
In some preferred embodiments, the first end of the exhaust tube extends into the reactor, and the wall of the first end of the exhaust tube extends obliquely outwards and upwards to form a horn-shaped structure.
Preferably, the included angle between the pipe wall of the first end of the exhaust pipe and the vertical direction is 30-60 degrees.
In a second aspect, the present invention provides a method for preparing a high-density polycrystalline silicon carbide rod, which is prepared by using the preparation device in the first aspect, wherein a negative pressure monitoring member monitors the pressure in a reactor, a pumping control part adjusts the pumping speed of a pumping part according to the pressure in the reactor, the pumping part pumps air from the reactor through a pumping pipe, the pressure in the reactor is kept at 0.001bar to 0.1bar, a deposition gas source is introduced into the reactor through a nozzle on a gas inlet pipe, and deposition reaction occurs on the surface of a deposition carrier to generate polycrystalline silicon carbide and hydrogen chloride gas.
In some preferred embodiments, when the pressure in the reactor is normal pressure, the total flow rate of the deposition gas source and the carrier gas is Q, and when the pressure in the reactor is kept at 0.001bar to 0.1bar, the total flow rate of the deposition gas source and the carrier gas is 0.08Q to 0.15Q.
In some preferred embodiments, the surface temperature of the deposition carrier is maintained at a preset temperature of 1200 ℃ to 1600 ℃ by energizing the deposition carrier through an electrode.
In some preferred embodiments, the pressure in the reactor is maintained at 0.01bar to 0.03bar.
In a third aspect, the invention provides a high-density polycrystalline silicon carbide rod prepared by the preparation method in the second aspect, wherein the density is more than 72%.
In a fourth aspect, the invention provides a high-purity polycrystalline silicon carbide powder, which is obtained by crushing the high-density polycrystalline silicon carbide rod in the third aspect.
According to the preparation device disclosed by the invention, the first end of the exhaust pipe is communicated with the inside of the reactor through the exhaust hole, the end part of the first end of the exhaust pipe is lower than the lower end of the deposition carrier, the second end of the exhaust pipe is communicated with the exhaust part, the exhaust control part is respectively connected with the negative pressure monitoring part and the exhaust part, and the negative pressure monitoring part monitors that the pressure of the reactor is not in the range of 0.001bar to 0.1bar, when the pressure of the reactor is not in the range of 0.001bar to 0.1bar, the exhaust speed of the exhaust part is adjusted, the pressure of the reactor is adjusted to be 0.001bar to 0.1bar, and as the pressure of the reactor can be kept to be 0.001bar to 0.1bar, the deposition process of depositing reaction of a deposition gas source to generate polycrystalline silicon carbide and hydrogen chloride gas can be improved, the flow rate of the gas on the surface of the deposition gas source is improved, the separation of reaction product hydrogen chloride and the surface of the polycrystalline silicon carbide rod is accelerated, the concentration of the hydrogen chloride gas in the reactor is reduced, so that on the one hand, corrosion of the polycrystalline silicon carbide rod by the hydrogen chloride gas on the polycrystalline silicon carbide rod is inhibited, the occurrence of corrosion of the polycrystalline silicon carbide rod is avoided, the silicon carbide rod, the occurrence of the hole and the coral-like structure on the silicon carbide rod is prevented, the deposition gas source is improved, and the deposition impurity deposition gas is promoted, and the deposition impurity is improved, and the deposition purity of the deposition gas source is on the polycrystalline silicon carbide rod. The invention improves the density of the polycrystalline silicon carbide rod by inhibiting the corrosion of the hydrogen chloride gas to the polycrystalline silicon carbide rod, and the polycrystalline silicon carbide rod with high density can further inhibit the corrosion of the hydrogen chloride gas.
According to the reactor of the preparation device, the pumping hole is formed in the center of the bottom plate, the vertical electrode penetrates through the bottom plate, the electrode is located outside the pumping hole, the upper end of the electrode is connected with the vertical deposition carrier, the air inlet hole is formed in the outer side of the electrode on the bottom plate, one end of the air inlet pipe extends to the inside of the reactor through the air inlet hole, the nozzle is arranged on the pipe section of the air inlet pipe located in the reactor, and the deposition reaction of a deposition air source entering from the air inlet pipe on the surface of the carrier is avoided on the basis that the pressure in the reactor is negative pressure, particularly 0.001bar-0.1 bar, and the negative pressure pumping is pumped out. Compared with the air inlet pipe which does not extend into the reactor, the air inlet pipe extends into the reactor, and the air flow is smoother and more stable under the double functions of the nozzle of the air inlet pipe extending into the reactor and the negative pressure, so that the deposited silicon carbide polycrystal deposited on the deposition carrier or the gas attached to all positions in the axial direction and the radial direction of the silicon carbide polycrystal is more uniform, and the deposited silicon carbide is more compact. The heat of the deposition carrier can be uniformly led out to the outermost layer along the deposited compact silicon carbide layer, and is matched with uniform air flow, so that the temperature of the surface layer is more uniform, and the compactness of the polycrystalline silicon carbide rod is further ensured.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural view of a production apparatus according to example 1 of the present invention.
Description of the reference numerals
1-Reactor, 11-base plate, 111-air pumping hole, 112-air inlet, 12-cover, 13-deposition carrier, 14-electrode, 2-air inlet pipe, 21-nozzle, 3-air pumping pipe and 31-horn structure.
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In this document, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used generally to refer to the orientation shown in the drawings and in the practice, and "inner" and "outer" are intended to refer to the interior and exterior of the outline of the component.
In the description of the present invention, it should be understood that the terms "center," "upper," "lower," "vertical," "horizontal," "top," "bottom," "inner," "outer," "axial," "radial," "circumferential," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the invention and simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "connected," "fixed" and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected or integrally formed, mechanically connected or electrically connected, directly connected or indirectly connected through an intermediate medium, or may be in communication with each other between two elements or in an interaction relationship between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.
The inventor of the invention researches and discovers that a polycrystalline silicon carbide rod is prepared by chemical vapor deposition of a silicon source gas and a carbon source gas on a carrier, more hole structures are easy to exist on the polycrystalline silicon carbide rod, the hole structures are easy to adsorb and mix impurities, and the purity of the polycrystalline silicon carbide powder is influenced after the polycrystalline silicon carbide rod is crushed.
In this regard, in a first aspect, the present invention provides an apparatus for preparing a high density polycrystalline silicon carbide rod, comprising:
The reactor 1 comprises a bottom plate 11, a cover body 12 covered on the bottom plate 11 and a vertical deposition carrier 13 positioned in the cover body 12, wherein an air suction hole 111 is formed in the center of the bottom plate 11, a vertical electrode 14 is arranged on the bottom plate 11 in a penetrating manner, the electrode 14 is positioned outside the air suction hole 111, the upper end of the electrode 14 is connected with the lower end of the deposition carrier 13, and an air inlet hole 112 is formed in the bottom plate 11 and positioned outside the electrode 14;
An air inlet pipe 2, wherein one end of the air inlet pipe 2 extends into the reactor 1 through the air inlet hole 112, and a nozzle 21 is arranged on a pipe section of the air inlet pipe 2 positioned in the reactor 1;
The negative pressure assembly comprises an exhaust pipe 3, an exhaust part, an exhaust control part and a negative pressure monitoring part, wherein a first end of the exhaust pipe 3 is communicated with the inside of the reactor 1 through an exhaust hole 111, the end part of the first end of the exhaust pipe 3 is lower than the lower end of the deposition carrier 13, a second end of the exhaust pipe 3 is communicated with the exhaust part, the negative pressure monitoring part monitors whether the pressure in the reactor 1 is in the range of 0.001bar-0.1bar, and the exhaust control part is respectively connected with the negative pressure monitoring part and the exhaust part;
One end of the air inlet pipe 2 extends to the upper part of the deposition carrier 13 through the air inlet hole 112, a plurality of nozzles 21 are arranged on the side part, close to the deposition carrier 13, of the pipe section of the air inlet pipe 2 positioned in the reactor 1, the nozzles 21 are arranged at intervals along the axial direction of the air inlet pipe 2, the uppermost nozzle 21 is positioned on the deposition carrier 13, and the lowermost nozzle 21 is positioned on the first end of the air exhaust pipe 3 and has a vertical distance of more than 50cm from the first end of the air exhaust pipe 3.
According to the preparation device of the invention, one end of the air inlet pipe 2 extends into the reactor 1 through the air inlet 112, carrier gas and deposition air source can be introduced into the reactor 1, a vertical electrode 14 is arranged on the bottom plate 11 of the reactor 1 in a penetrating way, the upper end of the electrode 14 is connected with the lower end of the vertical deposition carrier 13, the purpose of electrifying the deposition carrier 13 through the electrode 14 can be achieved, resistance heat is generated due to the resistance effect of the deposition carrier 13 after electrifying, the deposition air source flows through the surface of the deposition carrier 13 or the surface of silicon carbide polycrystal deposited on the deposition carrier 13, the deposition reaction grows into a polycrystalline silicon carbide rod, hydrogen chloride and other tail gases are generated during the deposition reaction, the negative pressure component comprises an exhaust pipe 3, an exhaust part, an exhaust control part and a negative pressure monitoring part, the first end of the exhaust pipe 3 is communicated with the interior of the reactor 1 through the exhaust hole 111, the second end of the exhaust pipe 3 is communicated with the exhaust part, the air extraction control part is respectively connected with the negative pressure monitoring piece and the air extraction part for monitoring whether the pressure in the reactor is in the range of 0.001bar-0.1 bar, so that when the negative pressure monitoring piece monitors that the pressure in the reactor 1 is not in the range of 0.001bar-0.1 bar, the air extraction control part adjusts the air extraction speed of the air extraction part, the pressure in the reactor 1 is quickly adjusted to be 0.001bar-0.1 bar, the pressure in the reactor 1 is kept to be 0.001bar-0.1 bar through air extraction, the gas flow rate on the surface of the polycrystalline silicon carbide rod can be improved, the separation of hydrogen chloride from the surface of the polycrystalline silicon carbide rod body is promoted, the concentration of hydrogen chloride gas in the reactor 1 can be reduced, and the concentration of the hydrogen chloride gas on the surface of the polycrystalline silicon carbide rod is reduced, so that on one hand, the corrosion of the hydrogen chloride gas on the polycrystalline silicon carbide rod can be inhibited, the occurrence of holes and coral-shaped structures on the silicon carbide rod due to the corrosion can be avoided, the compactness of the polycrystalline silicon carbide rod can be improved, the rod body is restrained from adsorbing impurity, the purity of the silicon carbide polycrystalline powder obtained after the polycrystalline silicon carbide rod is broken is improved, on the other hand, the deposition process of the deposition gas source for generating polycrystalline silicon carbide and hydrogen chloride gas through deposition reaction can be promoted, and the conversion rate of the deposition gas source is improved. The invention improves the density of the polycrystalline silicon carbide rod by inhibiting the corrosion of the hydrogen chloride gas to the polycrystalline silicon carbide rod, and the polycrystalline silicon carbide rod with high density can further inhibit the corrosion of the hydrogen chloride gas.
According to the preparation device disclosed by the invention, the air suction hole 111 is formed in the center of the bottom plate 11 of the reactor 1, the first end of the air suction pipe 3 is communicated with the inside of the reactor 1 through the air suction hole 111, the end part of the first end of the air suction pipe 3 is lower than the lower end of the deposition carrier 13, the vertical electrode 14 is arranged on the bottom plate 11 in a penetrating mode outside the air suction hole 111, the upper end of the electrode 14 is connected with the lower end of the vertical deposition carrier 13, the air suction hole 112 is formed in the outer side of the bottom plate 11, one end of the air suction pipe 2 extends to the inside of the reactor 1 through the air suction hole 112, the nozzle 21 is arranged on a pipe section of the air suction pipe 2, the air suction hole 111 is positioned on the inner side of the polycrystalline silicon carbide rod, the end part of the air suction pipe 3 is lower than the lower end of the deposition carrier 13, the air suction hole 112 is positioned on the periphery of the polycrystalline silicon carbide rod, a deposition air source and carrier gas are sprayed into the reactor 1 from the periphery of the polycrystalline silicon carbide rod, the deposition air source and the tail gas flows through the surface of the rod, the deposition air source, tail gas and the tail gas such as hydrogen chloride are brought out, the air suction pipe 3 at the lower part of the inner side of the polycrystalline silicon carbide rod is pumped away and the negative pressure of the air suction pipe 1 and the carrier 1 is prevented from being 0.0.0 bar to the deposition carrier 1bar and the deposition carrier gas can be further discharged from the surface to the deposition carrier 1. Meanwhile, compared with the fact that the air inlet pipe 2 does not extend into the reactor 1, the air flow is smoother and more stable under the double guiding effects of the nozzle 21 of the air inlet pipe 2 extending into the reactor 1 and negative pressure, so that the deposited carrier 13 or the gas attached to all positions of the deposited silicon carbide polycrystal in the axial direction and the radial direction on the deposited carrier 13 is more uniform, and the silicon carbide deposited on the surface layer is more compact. The heat of the deposition carrier 13 can be uniformly transferred by the compact silicon carbide, and the heat of the deposition carrier 13 can be uniformly led out to the surface layer along the deposited compact silicon carbide layer and matched with uniform air flow, so that the temperature of the surface layer is more uniform, and the compactness of the polycrystalline silicon carbide rod is further ensured.
The heat of the deposition carrier 13 can be unevenly transferred to the surface of the silicon carbide rod along with the formation of holes or coral-shaped silicon carbide, so that uneven temperature is further caused on the surface of the silicon carbide rod, silicon carbide cannot be well deposited at the place with relatively low temperature, larger holes or coral-shaped silicon carbide is further formed at the place, the further growth of the rod body is limited when serious, the growth diameter of the rod is further limited, the pressure of the reactor 1 is kept to be 0.001bar-0.1 bar, and the air inlet pipe 2 extends into the reactor 1 to form compact silicon carbide, so that the growth diameter of the rod body can be improved.
The air inlet pipe 2 extends to the upper part of the deposition carrier 13, the side part of the air inlet pipe 2, which is close to the deposition carrier 13, is provided with nozzles 21, the uppermost nozzle 21 is positioned above the deposition carrier 13, a deposition air source is sprayed to the deposition carrier 13 along the horizontal direction, a plurality of nozzles 21 are distributed along the height direction of the deposition carrier 13, and on the premise that the pressure in the reactor 1 is negative pressure, particularly 0.001bar-0.1 bar, the situation that the deposition air source entering from the air inlet pipe 2 does not reach the surface of the deposition carrier 13 is avoided, the negative pressure air suction is pumped out, the smooth and stable air flow is facilitated, the deposition air source is uniformly deposited on the deposition carrier 13, the deposition uniformity is improved, the compactness of polycrystalline silicon carbide rods is improved, and the vertical distance between the lowermost nozzle 21 and the first end of the air suction pipe 3 is more than 50cm, and the situation that the deposition air source sprayed out from the lowermost nozzle 21 does not reach the surface of the deposition carrier 13 is avoided, because the negative pressure air suction is pumped out.
It will be appreciated that the air intake holes 112 of the present invention are preferably uniformly disposed along the circumferential direction of the base plate 11.
In some preferred embodiments, the first end of the exhaust pipe 3 extends into the reactor 1, and the pipe wall of the first end of the exhaust pipe 3 extends obliquely upward and outward to form a horn-shaped structure 31. On the one hand, the deposition gas source needs to be fully circulated in the reactor 1 for full deposition, on the other hand, the gases such as hydrogen chloride and the like need to be rapidly discharged to inhibit corrosion, and the rapid discharge of the gases such as hydrogen chloride and the like through the exhaust pipe 3 also brings about the discharge of the deposition gas source, under the preferred scheme, the first end of the exhaust pipe 3 is in a horn-shaped structure 31, the tail gas containing the hydrogen chloride component with higher concentration in the central area can be effectively collected, the gases such as hydrogen chloride and the like are promoted to be rapidly and stably extracted from the reactor 1, the invention is more beneficial to balancing the effects of full deposition of a deposition gas source and rapid discharge of gases such as hydrogen chloride to inhibit corrosion, and can control the hydrogen chloride to corrode the polycrystalline silicon carbide rod while maintaining good utilization rate of the deposition gas, so that the polycrystalline silicon carbide rod has good compactness.
Preferably, the included angle between the pipe wall of the first end of the exhaust pipe 3 and the vertical direction is 30-60 degrees. Under the preferred scheme, the method is more beneficial to balancing the effects of full deposition of a deposition gas source and rapid discharge of gases such as hydrogen chloride and the like to inhibit corrosion.
In some preferred embodiments, the negative pressure monitoring part monitors whether the pressure in the reactor 1 is within the range of 0.01bar to 0.03bar, which is more beneficial to inhibiting the corrosion of the hydrogen chloride gas to the polycrystalline silicon carbide rod, improving the compactness of the polycrystalline silicon carbide rod, improving the purity of the polycrystalline silicon carbide powder and improving the conversion rate of a deposition gas source.
In a second aspect, the present invention provides a method for preparing a high-density polycrystalline silicon carbide rod, which is prepared by using the preparation device in the first aspect, wherein a negative pressure monitoring member monitors the pressure in the reactor 1, a pumping control part adjusts the pumping speed of a pumping part according to the pressure in the reactor 1, the pumping part pumps air from the reactor 1 through a pumping pipe 3, the pressure in the reactor 1 is kept at 0.001bar to 0.1bar, a deposition air source is introduced into the reactor 1 through a nozzle 21 on an air inlet pipe 2, and deposition reaction occurs on the surface of a deposition carrier 13 to generate polycrystalline silicon carbide and hydrogen chloride gas.
According to the preparation method, the negative pressure monitoring piece monitors the pressure in the reactor 1, the air extraction control part adjusts the air extraction speed of the air extraction part according to the pressure in the reactor 1, the air extraction part extracts air from the reactor 1, the pressure in the reactor 1 is kept to be 0.001 bar-0.1 bar, the gas flow rate of the surface of the polycrystalline silicon carbide rod can be improved, the separation of hydrogen chloride and the surface of the polycrystalline silicon carbide rod body is promoted, the concentration of the hydrogen chloride gas in the reactor 1 can be reduced, the concentration of the hydrogen chloride gas on the surface of the polycrystalline silicon carbide rod is reduced, the corrosion of the hydrogen chloride gas on the polycrystalline silicon carbide rod is further inhibited, holes and coral-shaped structures on the silicon carbide rod are avoided, the compactness of the polycrystalline silicon carbide rod is improved, the impurity absorption of the rod body is inhibited, and the purity of the polycrystalline silicon carbide polycrystalline powder obtained after the polycrystalline silicon carbide rod is broken is improved. The pressure in the reactor 1 is kept at 0.001bar-0.1 bar, the generation of particles in the atmosphere in the reactor 1 can be restrained, the utilization rate of raw material gas is improved, and the pipeline blockage caused by the particles carried in the gas entering the exhaust pipe 3 is prevented.
If the pressure in the reactor 1 is lower than 0.001bar, the problem that the growth speed of the silicon carbide polycrystal is too slow is easily caused, for example, the growth speed can only reach the order of microns per hour, for example, a silicon carbide film is difficult to grow into a silicon carbide rod, while if the growth speed is higher than 0.1bar, the problem that hydrogen chloride is easily accumulated on the surface of the polycrystalline silicon carbide rod and corrodes the polycrystalline silicon carbide rod is easily caused.
The deposition gas source is not limited in the invention, and the deposition gas source can be at least one of mixed gas of SiCH 3Cl3、CH4 and SiCl 4 and mixed gas of SiH 4 and CCl 4. The type of the carrier gas is not limited, and the carrier gas can be at least one of hydrogen and argon, and the pressure in the reactor is kept at 0.001bar-0.1 bar, so that the separation of hydrogen chloride from the surface of the polycrystalline silicon carbide rod body can be promoted, the concentration of the hydrogen chloride gas on the surface of the polycrystalline silicon carbide rod body can be reduced, and the corrosion of the hydrogen chloride on the silicon carbide rod can be inhibited when the carrier gas adopts hydrogen.
The pressure in the reactor 1 according to the invention can be maintained, for example, at 0.001bar, 0.003bar, 0.005bar, 0.008bar, 0.01bar, 0.03bar, 0.05bar, 0.07bar, 0.09bar and 0.1bar.
In some preferred embodiments, when the pressure in the reactor 1 is normal pressure, the total flow rate of the deposition gas source and the carrier gas is Q, and when the pressure in the reactor 1 is kept at 0.001bar to 0.1bar, the total flow rate of the deposition gas source and the carrier gas is 0.08Q to 0.15Q. Under the preferred scheme, the total flow of the deposition gas source and the carrier gas is 8% -15% of the normal pressure total flow, so that the excessive deposition speed caused by the excessive high concentration of the deposition gas source on the surface of the rod body can be prevented, the occurrence of holes and coral structures on the silicon carbide rod can be more favorably restrained, the compactness of the polycrystalline silicon carbide rod is improved, the adsorption of impurities in the rod body is restrained, the deposition process of the deposition gas source for generating polycrystalline silicon carbide and hydrogen chloride gas through the deposition reaction can be promoted because the pressure in the reactor 1 is kept to be 0.001bar-0.1 bar, the conversion rate of the deposition gas source is improved, and the good deposition speed can still be kept and the deposition is stabilized when the total flow of the deposition gas source and the carrier gas is 8% -15% of the normal pressure total flow. When the pressure in the reactor 1 is normal pressure, the same material flow rate on the surface of the silicon carbide rod body is achieved, and the total flow of the deposition gas source and the carrier gas can be obtained by means of historical data, theoretical calculation and the like. Preferably, when the pressure in the reactor 1 is kept at 0.001bar to 0.1bar, the total flow rate of the deposition gas source and the carrier gas is 0.12q to 0.15q.
In some preferred embodiments, the surface temperature of the deposition carrier 13 is maintained at a preset temperature of 1200 ℃ to 1600 ℃ by energizing the deposition carrier 13 through the electrode 14. Under the preferred scheme, the temperature of the surface of the deposition carrier 13 is 1200-1600 ℃, the temperature is relatively high, the conversion rate of a deposition air source can be further improved, when the total flow of the deposition air source and carrier gas is 8-15% of the total flow of normal pressure, the better deposition speed is better kept, the deposition is stabilized, the pressure in the reactor 1 is kept to be 0.001bar-0.1 bar, the separation speed of hydrogen chloride generated by the deposition reaction and the surface of the polycrystalline silicon carbide rod body is high, the concentration of the hydrogen chloride gas on the surface of the polycrystalline silicon carbide rod is low, and even if the relatively high deposition temperature of 1200-1600 ℃ is adopted, the corrosion of the hydrogen chloride gas to the polycrystalline silicon carbide rod can be effectively controlled, and the compactness of the silicon carbide rod is ensured. Preferably, the preset temperature is 1450-1600 ℃.
In some preferred embodiments, the pressure in the reactor 1 is kept at 0.01 bar-0.03 bar, which is more beneficial to inhibiting the corrosion of hydrogen chloride gas to the polycrystalline silicon carbide rod, improving the compactness of the polycrystalline silicon carbide rod, improving the purity of the polycrystalline silicon carbide powder and improving the conversion rate of a deposition gas source.
In some preferred embodiments, the deposition gas source is ejected through the nozzle 21 on the gas inlet pipe 2 at a flow rate of 5m/s to 50m/s.
In some preferred embodiments, before the deposition gas source is introduced into the reactor 1, a carrier gas is introduced into the reactor 1 to replace the atmosphere in the reactor 1, the impurity atmosphere such as air, water vapor and the like in the reactor 1 is removed, the deposition gas source and the carrier gas are mixed and then introduced into the reactor 1 through the gas inlet pipe 2, the gas pumped by the pumping part is subjected to tail gas recovery, the tail gas recovery comprises pressurization, cooling, segregation, rectification and the like, and the deposition gas source and the carrier gas obtained by purification are sent into the reactor 1 again.
In a third aspect, the invention provides a high-density polycrystalline silicon carbide rod prepared by the preparation method in the second aspect, wherein the density is more than 72%.
In a fourth aspect, the invention provides a high-purity polycrystalline silicon carbide powder, which is obtained by crushing the high-density polycrystalline silicon carbide rod in the third aspect.
The invention will be further described in detail with reference to specific examples.
Example 1
The preparation device of the high-density polycrystalline silicon carbide rod is shown in FIG. 1 (the arrow lines in FIG. 1 indicate the flow directions of a deposition gas source and a carrier gas), and comprises a reactor 1, an air inlet pipe 2 and a negative pressure component; the reactor 1 comprises a bottom plate 11 and a cover body 12 covered on the bottom plate 11, a vertical deposition carrier 13 is arranged in the cover body 12, an air suction hole 111 is arranged in the center of the bottom plate 11, a vertical electrode 14 is arranged on the bottom plate 11 in a penetrating mode, the electrode 14 is positioned outside the air suction hole 111, the upper end of the electrode 14 is connected with the lower end of the deposition carrier 13, an air inlet 112 is arranged on the outer side of the electrode 14 on the bottom plate 11, one end of an air inlet pipe 2 extends to the upper portion of the deposition carrier 13 through the air inlet 112, a nozzle 21 is arranged on the side portion, close to the deposition carrier 13, of the inner part of the air inlet pipe 2, the uppermost nozzle 21 is arranged on the deposition carrier 13 at intervals along the axial direction of the air inlet pipe 2, a negative pressure component comprises an air suction pipe 3, an air suction part (not shown), an air suction control part (not shown in the drawing), and a negative pressure monitoring part (not shown in the drawing), a first end of the air suction pipe 3 is communicated with the inner part of the reactor 1 through the air suction hole 111 and extends to the inner part of the reactor 1, the wall of the first end of the air suction pipe 3 is inclined upwards to form a horn-shaped structure 31, the wall of the first end of the air suction pipe 3 is inclined outwards, the first end is connected with the lower end of the air suction pipe 30 DEG, and the air suction pipe 3 is communicated with the lower end of the air suction pipe 3 is communicated with the lower end of the air end 30, the air extraction control part is respectively connected with a negative pressure monitoring part and an air extraction part for monitoring whether the pressure in the reactor 1 is in the range of 0.01 bar-0.03bar, and the nozzle 21 at the lowest end is positioned above the first end of the air extraction pipe 3 and has a vertical distance of 60cm with the first end of the air extraction pipe 3.
The preparation method of the high-density polycrystalline silicon carbide rod adopts the preparation device to prepare, and comprises the following steps:
The connection of the exhaust pipe 3 and the exhaust part is disconnected, hydrogen (carrier gas) and argon (carrier gas) are introduced into the reactor 1 through the air inlet pipe 2, the atmosphere in the cavity of the reactor 1 is discharged from the exhaust pipe 3, the replacement of the atmosphere in the cavity of the reactor 1 is realized, and the pressure in the reactor 1 is normal pressure after the replacement;
step 2, connecting an exhaust pipe 3 with an exhaust part, enabling a negative pressure monitoring piece to monitor the pressure in the reactor 1, exhausting air through the exhaust part to enable the pressure in the reactor 1 to be 0.01 bar-0.03 bar, electrifying the deposition carrier 13 by using an electrode 14, generating resistance heat due to the self resistance effect after electrifying the deposition carrier 13, and enabling the surface temperature of the deposition carrier 13 to be 1600 ℃;
Step 3, siCH 3Cl3 (deposition air source), hydrogen (carrier gas) and argon (carrier gas) are mixed and then are introduced into the reactor 1 through the air inlet pipe 2, the mixture flows to the surface of the deposition carrier 13 to react to generate silicon carbide polycrystal and hydrogen chloride gas, when the total flow of the deposition air source and the carrier gas is 0.12Q and the pressure in the reactor 1 is normal pressure, the total flow of the deposition air source and the carrier gas is monitored by the negative pressure monitoring piece in the ventilation process, the air suction speed of the air suction part is regulated by the air suction control part according to the pressure in the reactor 1, the air suction part sucks air from the reactor 1 through the air suction pipe 3, the pressure in the reactor 1 is kept to be 0.01-0.03 bar, tail gas recovery is carried out on the air sucked by the air suction part, and the purified SiCH 3Cl3, the hydrogen and the argon are returned for reuse after pressurization, cooling, segregation, rectification and the like.
Example 2
Reference is made to example 1, which differs in that the wall of the first end of the extraction tube 3 of the preparation device is at an angle of 15 ° to the vertical.
Example 3
Referring to example 1, the difference is that the first end of the exhaust pipe 3 of the preparation apparatus does not extend into the reactor 1, the first end of the exhaust pipe 3 is flush with the bottom plate 11, and the first end of the exhaust pipe 3 does not form the horn-like structure 31.
Example 4
Reference is made to example 1, which differs in that the total flow of deposition source and carrier gas is 0.5Q in step 3 of the preparation method.
Example 5
Referring to example 1, the difference is that in step 2 of the preparation method, the negative pressure monitoring member monitors the pressure in the reactor 1, the pressure in the reactor 1 is 0.05bar to 0.1bar by pumping air through the pumping air part, and in step 3, the pressure in the reactor 1 is maintained to be 0.05bar to 0.1bar, and the negative pressure monitoring member of the preparation device monitors whether the pressure in the reactor 1 is in the range of 0.05bar to 0.1 bar.
Comparative example 1
Referring to example 1, the difference is that in step 2 of the production method, the negative pressure monitoring means monitors the pressure in the reactor 1, the pressure in the reactor 1 is 1.0bar to 1.2b ar by pumping air from the pumping section, and in step 3, the pressure in the reactor 1 is maintained at 1.0bar to 1.2b ar, and the negative pressure monitoring means of the production apparatus monitors whether the pressure in the reactor 1 is within the range of 1.0bar to 1.2b ar.
Test case
The densities of the polycrystalline silicon carbide rods prepared by the preparation methods of examples 1-5 and comparative example 1 are measured, the polycrystalline silicon carbide rods are crushed into small fragments with the particle size of 10 mm-30 mm, the depth of pits on the surfaces of the small fragments is measured, small fragments with pit depths of more than 5mm and small fragments with pit depths of less than 5mm are separated, and the proportion of the weight of the small fragments with pit depths of less than 5mm to the weight of the polycrystalline silicon carbide rods is calculated to obtain the density. The polycrystalline silicon carbide rods prepared by the preparation methods of examples 1 to 5 and comparative example 1 were crushed to obtain polycrystalline silicon carbide powder, the impurity element content of the polycrystalline silicon carbide powder was measured by Glow Discharge Mass Spectrometry (GDMS) and Secondary Ion Mass Spectrometry (SIMS) with reference to GB/T37254-2018 and GB/T41153-2021, and the purity of the polycrystalline silicon carbide powder was obtained after removing the impurity element content, as shown in Table 1. The purity of the table is >7.5N, which represents purity of more than 99.999995%, purity of >7N, purity of more than 99.99999%, purity of >6N, and purity of more than 99.9999%.
TABLE 1
In the comparative examples and comparative examples, the pressure in the reactor 1 is kept at 0.001bar to 0.1bar, so that the compactness of the polycrystalline silicon carbide rod can be improved, and the purity of the polycrystalline silicon carbide powder can be improved.
In comparative examples 1 to 3, it can be known that the first end of the exhaust tube 3 extends into the reactor 1, and the tube wall of the first end of the exhaust tube 3 extends obliquely upward outwards to form a horn-shaped structure 31, which is more beneficial to improving the density of the polycrystalline silicon carbide rod, and the included angle between the tube wall of the first end of the exhaust tube 3 and the vertical direction is 30 ° to 60 °, which is more beneficial to further improving the density of the polycrystalline silicon carbide rod. In comparative examples 1 and 4, the total flow of the deposition gas source and the carrier gas is 0.08Q-0.15Q, which is more beneficial to improving the density of the polycrystalline silicon carbide rod and improving the purity of the polycrystalline silicon carbide powder. In the comparative examples 1 and 5, the pressure in the reactor 1 is kept at 0.01 bar-0.03 bar, which is more beneficial to improving the compactness of the polycrystalline silicon carbide rod and improving the purity of the polycrystalline silicon carbide powder.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (9)
1. The utility model provides a preparation facilities of high density polycrystalline silicon carbide stick which characterized in that includes:
The reactor (1), reactor (1) include bottom plate (11), cover body (12) and being located on the bottom plate (11) cover body (13) inside vertical deposition carrier of cover body (12), the central authorities of bottom plate (11) are provided with gas vent (111), wear to be equipped with vertical electrode (14) on bottom plate (11), electrode (14) are located the outside of gas vent (111), the upper end of electrode (14) with the lower extreme of deposition carrier (13) is connected, be provided with inlet port (112) on bottom plate (11) are located the outside of electrode (14);
The air inlet pipe (2), one end of the air inlet pipe (2) extends to the inside of the reactor (1) through the air inlet hole (112), and a nozzle (21) is arranged on a pipe section of the air inlet pipe (2) positioned in the inside of the reactor (1);
The negative pressure assembly comprises an exhaust pipe (3), an exhaust part, an exhaust control part and a negative pressure monitoring piece, wherein a first end of the exhaust pipe (3) is communicated with the inside of the reactor (1) through an exhaust hole (111), the end part of the first end of the exhaust pipe (3) is lower than the lower end of the deposition carrier (13), a second end of the exhaust pipe (3) is communicated with the exhaust part, the negative pressure monitoring piece monitors whether the pressure in the reactor (1) is in the range of 0.001bar-0.1 bar, and the exhaust control part is respectively connected with the negative pressure monitoring piece and the exhaust part;
One end of the air inlet pipe (2) extends to the upper part of the deposition carrier (13) through the air inlet hole (112), a plurality of nozzles (21) are arranged on the side part, close to the deposition carrier (13), of the pipe section inside the reactor (1) of the air inlet pipe (2), the nozzles (21) are arranged along the axial interval of the air inlet pipe (2), the uppermost nozzle (21) is positioned on the deposition carrier (13), and the lowermost nozzle (21) is positioned on the first end of the exhaust pipe (3) and is more than 50cm in vertical distance from the first end of the exhaust pipe (3).
2. The preparation device of the high-density polycrystalline silicon carbide rod according to claim 1, wherein the first end of the exhaust tube (3) extends into the reactor (1), and the tube wall of the first end of the exhaust tube (3) extends outwards and upwards in an inclined manner to form a horn-shaped structure (31).
3. The preparation device of the high-density polycrystalline silicon carbide rod according to claim 2, wherein an included angle between the pipe wall of the first end of the exhaust pipe (3) and the vertical direction is 30-60 degrees.
4. The preparation method of the high-density polycrystalline silicon carbide rod is characterized in that the preparation device of the high-density polycrystalline silicon carbide rod is characterized in that a negative pressure monitoring piece is used for monitoring the pressure in a reactor (1), an air extraction control part is used for adjusting the air extraction speed of an air extraction part according to the pressure in the reactor (1), the air extraction part is used for extracting air from the reactor (1) through an air extraction pipe (3), the pressure in the reactor (1) is kept to be 0.001bar-0.1 bar, a deposition air source is introduced into the reactor (1) through a nozzle (21) on an air inlet pipe (2), and deposition reaction is carried out on the surface of a deposition carrier (13) to generate polycrystalline silicon carbide and hydrogen chloride gas.
5. The method for preparing the high-density polycrystalline silicon carbide rod according to claim 4, wherein when the pressure in the reactor (1) is normal pressure, the total flow rate of the deposition gas source and the carrier gas is Q, and when the pressure in the reactor (1) is kept at 0.001bar-0.1 bar, the total flow rate of the deposition gas source and the carrier gas is 0.08Q-0.15Q.
6. The method for preparing a high-density polycrystalline silicon carbide rod according to claim 4 or 5, characterized in that the surface temperature of the deposition carrier (13) is kept at a preset temperature of 1200-1600 ℃ by electrifying the deposition carrier (13) through an electrode (14).
7. The method for producing a high-density polycrystalline silicon carbide rod according to claim 4, wherein the pressure in the reactor (1) is kept at 0.01bar to 0.03bar.
8. A high-density polycrystalline silicon carbide rod prepared by the method for preparing a high-density polycrystalline silicon carbide rod according to any one of claims 4 to 7, characterized in that the density is 72% or more.
9. A high purity polycrystalline silicon carbide powder obtained by crushing the high density polycrystalline silicon carbide rod of claim 8.
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