CN114657632B - Tantalum structure, temperature measuring hole structure, crucible assembly and temperature measuring hole anti-blocking method - Google Patents
Tantalum structure, temperature measuring hole structure, crucible assembly and temperature measuring hole anti-blocking method Download PDFInfo
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- CN114657632B CN114657632B CN202210173332.4A CN202210173332A CN114657632B CN 114657632 B CN114657632 B CN 114657632B CN 202210173332 A CN202210173332 A CN 202210173332A CN 114657632 B CN114657632 B CN 114657632B
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical group [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 25
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 71
- 239000013078 crystal Substances 0.000 claims abstract description 45
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910003468 tantalcarbide Inorganic materials 0.000 claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 19
- 239000010439 graphite Substances 0.000 claims abstract description 19
- 238000000859 sublimation Methods 0.000 claims abstract description 15
- 230000008022 sublimation Effects 0.000 claims abstract description 15
- 238000009529 body temperature measurement Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 3
- 229910052735 hafnium Inorganic materials 0.000 claims description 3
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- 239000010955 niobium Substances 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 239000010937 tungsten Substances 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 25
- 229910052710 silicon Inorganic materials 0.000 abstract description 25
- 239000010703 silicon Substances 0.000 abstract description 25
- 239000007789 gas Substances 0.000 abstract description 22
- 230000007797 corrosion Effects 0.000 abstract description 14
- 238000005260 corrosion Methods 0.000 abstract description 14
- 230000008018 melting Effects 0.000 abstract description 11
- 238000002844 melting Methods 0.000 abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 10
- 230000006911 nucleation Effects 0.000 abstract description 10
- 238000010899 nucleation Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 10
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
Classifications
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/60—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes
- C23C8/62—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using solids, e.g. powders, pastes only one element being applied
- C23C8/64—Carburising
-
- 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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention relates to the technical field of silicon carbide crystal preparation, and discloses a tantalum structure, a preparation method of the tantalum structure, a temperature measuring hole structure, a crucible assembly, a temperature measuring hole anti-blocking method and a silicon carbide crystal preparation method. Wherein, the crucible assembly includes: the crucible comprises a crucible body and a crucible cover; the crucible body is made of first graphite and comprises an upper crucible section and a lower crucible section which are detachably connected with each other; the crucible cover is made of second graphite, is detachably connected with the crucible body and forms an accommodating cavity with the crucible body; and the temperature measuring hole structures are arranged at the upper end and the lower end of the crucible. Through the technical scheme, the characteristic that the melting point of the tantalum carbide is higher than the sublimation temperature of the silicon carbide is utilized, the tantalum carbide has chemical inertness to silicon and hydrogen at high temperature, the corrosion of silicon-rich gas to the inner wall of a tantalum structure is effectively avoided, the silicon carbide is prevented from being generated in the temperature measuring holes, a large number of nucleation points cannot be provided for the subsequent growth of the silicon carbide, and the blockage of the temperature measuring holes is avoided.
Description
Technical Field
The invention relates to the technical field of silicon carbide crystal preparation, in particular to a tantalum structure, a preparation method of the tantalum structure, a temperature measuring hole structure, a crucible assembly, a temperature measuring hole anti-blocking method and a silicon carbide crystal preparation method.
Background
A wide band gap semiconductor material represented by silicon carbide (SiC) and gallium nitride (GaN) is a third generation wide band gap semiconductor subsequent to silicon (Si), gallium arsenide (GaAs). Compared with the traditional semiconductor materials represented by Si and GaAs, siC has great advantages in the aspects of working temperature, radiation resistance, breakdown voltage resistance and the like, and as the most mature wide band gap semiconductor material developed at present, siC has the advantages of high thermal conductivity, high breakdown field strength, high saturated electron drift rate, high bonding energy and the like, and the excellent performance can meet the new requirements of modern electronic technology on high temperature, high frequency, high power and radiation resistance, and has wide application requirements in the fields of LED illumination, electric energy conversion, radar communication and the like, so the SiC is regarded as one of the most promising materials in the field of semiconductor materials.
Currently, in the aspect of silicon carbide crystal growth, a high temperature sublimation method of seed crystal is mainly adopted, which is also called a Physical Vapor Transport (PVT) method. In a method for growing silicon carbide crystals by PVT, a graphite crucible is used for loading seed crystals and silicon carbide raw materials, fibrous heat preservation layers such as carbon-based soft felt, hard felt and the like are wrapped outside the graphite crucible, and temperature measurement holes are needed to be formed in the centers of the top heat preservation layer and the bottom heat preservation layer for monitoring the temperature of the crucible. When growing silicon carbide crystals, the feedstock needs to be heated to a temperature above 2200 c while the seed is controlled to a slightly lower temperature, the feedstock sublimates from the feedstock zone, and the feedstock sublimates to a single crystal at the seed. In the growth process of silicon carbide crystals, as the graphite crucible is of a pore structure, gas in the crucible can continuously overflow, and the silicon-rich atmosphere can corrode carbon materials outside the crucible and react with the carbon materials to generate silicon carbide, particularly at gas channels such as upper and lower temperature measuring holes, the generation of the silicon carbide is particularly rapid, the temperature measurement Kong Ji is easy to be blocked, the temperature control is invalid, and the high-quality growth of the crystals is further affected.
Disclosure of Invention
The invention aims to solve the defects of failure temperature control and low crystal growth quality of the existing PVT grown silicon carbide crystal, and provides a tantalum structure, a preparation method of the tantalum structure, a temperature measuring hole structure, a crucible assembly, an anti-blocking method of the temperature measuring hole and a preparation method of the silicon carbide crystal, so as to ensure the accuracy and stability of temperature monitoring in the crystal growth process.
In order to achieve the above object, a first aspect of the present invention provides a tantalum structure comprising a first body and a tantalum carbide layer covering the first body; wherein the first body is made of any one or more metals of hafnium, niobium, zirconium and tungsten.
Through the technical scheme, when the tantalum structure is installed in the temperature measuring hole, the characteristic that the melting point of tantalum carbide is higher than the sublimation temperature of silicon carbide is utilized, and the tantalum carbide has chemical inertness to silicon and hydrogen at high temperature, so that the corrosion of silicon-rich gas to the inner wall of the tantalum structure can be effectively avoided, the silicon carbide is prevented from being generated in the temperature measuring hole, a large number of nucleation points cannot be provided for subsequent growth of the silicon carbide, and the blockage of the temperature measuring hole is avoided.
The second aspect of the present invention provides a method for preparing a tantalum structure, which is characterized in that the method comprises: the first body is buried in carbon powder and subjected to high-temperature sintering treatment at a temperature of 2400 ℃ or higher, so that a tantalum carbide layer is formed on the outer surface of the first body.
According to the technical scheme, the tantalum structure prepared by the method has the characteristics of high melting point, corrosion resistance and chemical inertness to silicon and hydrogen at high temperature. When the tantalum structure is arranged in a temperature measuring hole formed in a graphite crucible for growing silicon carbide crystals, the corrosion of silicon-rich gas to the inner wall of the tantalum structure can be effectively avoided, silicon carbide is prevented from being formed in the temperature measuring hole, and the blockage of the temperature measuring hole is avoided.
A third aspect of the present invention provides a temperature measurement hole structure, comprising:
a second body;
a temperature measuring hole penetrating through the second body;
the tantalum structure or the tantalum structure obtained by the preparation method is arranged in the temperature measuring hole and covers the inner wall of the temperature measuring hole.
Through the technical scheme, when the tantalum structure is installed in the temperature measuring hole, the characteristic that the melting point of tantalum carbide is higher than the sublimation temperature of silicon carbide is utilized, and the tantalum carbide has chemical inertness to silicon and hydrogen at high temperature, so that the corrosion of silicon-rich gas to the inner wall of the tantalum structure is effectively avoided, silicon carbide is prevented from being generated in the temperature measuring hole, a large number of nucleation points cannot be provided for subsequent growth of silicon carbide, and the blockage of the temperature measuring hole is avoided.
Further, the second body is a hard felt.
A fourth aspect of the present invention provides a crucible assembly, comprising:
the crucible comprises a crucible body and a crucible cover; the crucible body is made of first graphite and comprises an upper crucible section and a lower crucible section which are detachably connected with each other; the crucible cover is made of second graphite, is detachably connected with the crucible body and forms an accommodating cavity with the crucible body.
And the temperature measuring hole structures are arranged at the upper end and the lower end of the crucible.
Through the technical scheme, the characteristic that the melting point of the tantalum carbide is higher than the sublimation temperature of the silicon carbide is utilized, the tantalum carbide has chemical inertness to silicon and hydrogen at high temperature, the corrosion of silicon-rich gas to the inner wall of a tantalum structure is effectively avoided, the silicon carbide is prevented from being generated in the temperature measuring holes, a large number of nucleation points cannot be provided for the subsequent growth of the silicon carbide, and the blockage of the temperature measuring holes is avoided.
Further, the second graphite has a porosity less than the first graphite.
Further, the crucible cover is in threaded connection with the crucible body; the upper section of the crucible is connected with the lower section of the crucible through threads.
Further, a first internal thread is arranged at the joint of the crucible cover and the crucible upper section; the joint of the upper section of the crucible and the crucible cover is provided with a first external thread which is matched with the first internal thread; a second internal thread is arranged at the joint of the upper section of the crucible and the lower section of the crucible; the joint of the crucible lower section and the crucible upper section is provided with a second external thread which is matched with the second internal thread; the first and second internal threads have a lower coefficient of thermal expansion than the first and second external threads.
Further, the crucible further comprises an insulating layer, and the insulating layer wraps the periphery of the crucible.
Further, the heat preservation layer is soft felt.
In a fifth aspect, the present invention provides a method for preventing clogging of a temperature measuring hole, the method comprising using the crucible assembly so as to prevent clogging of a gas sublimated from a raw material region in the temperature measuring hole when preparing a silicon carbide crystal.
Through the technical scheme, the characteristic that the melting point of the tantalum carbide is higher than the sublimation temperature of the silicon carbide is utilized, the tantalum carbide has chemical inertness to silicon and hydrogen at high temperature, the corrosion of silicon-rich gas to the inner wall of a tantalum structure is effectively avoided, the silicon carbide is prevented from being generated in the temperature measuring holes, a large number of nucleation points cannot be provided for the subsequent growth of the silicon carbide, and the blockage of the temperature measuring holes is avoided.
The sixth aspect of the present invention provides a method for producing a silicon carbide crystal, comprising the crucible assembly, the method comprising:
loading a proper amount of silicon carbide powder in the accommodating cavity;
placing seed crystals on the lower end face of the crucible cover;
and heating the silicon carbide powder to the sublimation temperature of silicon carbide, and simultaneously controlling the temperature near the seed crystal to be lower than the sublimation temperature so as to enable the silicon carbide gas to be sublimated at the seed crystal to obtain silicon carbide crystals.
Through the technical scheme, the temperature measuring holes can be prevented from being blocked, so that accurate temperature is obtained, accurate data basis is provided for preparing silicon carbide crystal, and the silicon carbide crystal with better quality is prepared.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
FIG. 1 is a schematic diagram of one embodiment of a tantalum structure of the present invention;
FIG. 2 is a schematic diagram of an embodiment of a temperature sensing orifice structure according to the present invention;
FIG. 3 is a schematic view of the structure of one embodiment of a crucible assembly of the present invention;
FIG. 4 is an exploded view of FIG. 3;
FIG. 5 is a schematic view of another embodiment of a crucible assembly of the present invention.
Description of the reference numerals
10 a first body; a second body 20; 30 temperature measuring holes; a 40 tantalum structure; 51 crucible body; 52 crucible cover; 53 crucible cutting; 54 crucible lower section; 53a first external thread; 53b second internal threads; 54a second external threads; 60 accommodating cavities; 70 insulating layer.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
In the present invention, unless otherwise indicated, terms of orientation such as "upper and lower" are used to generally refer to orientations in the assembled state of use. "inner and outer" means inner and outer relative to the contour of the respective parts themselves.
A first aspect of the present invention provides a tantalum structure, as shown in fig. 1, comprising a first body 10 and a tantalum carbide layer (not shown in the drawings) overlying the first body 10; wherein the first body 10 is made of any one or more metals of hafnium, niobium, zirconium and tungsten.
When the tantalum structure is installed in the temperature measuring hole, the characteristic that the melting point of tantalum carbide (3730-3830 ℃) is higher than the sublimation temperature of silicon carbide is utilized, and the tantalum carbide has chemical inertness to the growth of silicon and hydrogen high-purity semi-insulating silicon carbide crystals at high temperature. When the silicon-rich gas flows through the tantalum structure, the corrosion of the silicon-rich gas to the tantalum structure can be effectively avoided, so that silicon carbide is prevented from being generated in the temperature measuring holes, a large number of nucleation points cannot be provided for subsequent growth of the silicon carbide, and the blockage of the temperature measuring holes is avoided.
The second aspect of the present invention provides a method for manufacturing a tantalum structure, the method comprising: the first body 10 is buried in carbon powder and subjected to high-temperature sintering treatment at 2400 ℃ or higher, so that the outer surface of the first body 10 forms a tantalum carbide layer. The first body 10 is sintered at a high temperature above 2400 ℃ to form a tantalum carbide layer on the outer surface of the first body 10, and the melting point of tantalum carbide is between 3730 ℃ and 3830 ℃ and is obviously higher than the sublimation temperature of silicon carbide. The tantalum structure prepared by the method has the characteristics of high melting point, corrosion resistance and chemical inertness to the growth of silicon and hydrogen high-purity semi-insulating silicon carbide crystals at high temperature. When the tantalum structure is arranged in the temperature measuring hole, the corrosion of the silicon-rich gas to the inner wall of the tantalum structure can be effectively avoided, silicon carbide is prevented from being formed in the temperature measuring hole, a large number of nucleation points are not provided for subsequent growth of the silicon carbide, and thus the blockage of the temperature measuring hole is avoided
A third aspect of the present invention provides a temperature measuring hole structure, as shown in fig. 2, comprising:
a second body 20;
a temperature measuring hole 30 penetrating the second body 20;
and the tantalum structure 40 is arranged in the temperature measuring hole 30 and covers the inner wall of the temperature measuring hole 30.
Through the above technical scheme, when the tantalum structure 40 is installed in the temperature measuring hole 30, based on the characteristics of the tantalum structure 40, the corrosion of the silicon-rich gas to the inner wall of the tantalum structure can be effectively avoided, and silicon carbide is prevented from being generated in the temperature measuring hole, so that a large number of nucleation points cannot be provided for subsequent growth of the silicon carbide, and the blockage of the temperature measuring hole is avoided.
In an alternative embodiment, the second body 20 is a hard felt.
A fourth aspect of the present invention provides a crucible assembly, as shown in fig. 3 and 4, comprising:
a crucible including a crucible body 51 and a crucible cover 52; wherein the crucible body 51 is made of first graphite, and the crucible body 51 comprises a crucible upper section 53 and a crucible lower section 54 which are detachably connected with each other; the crucible cover 52 is made of second graphite, is detachably connected with the crucible body 51, and forms a containing cavity 60 with the crucible body 51.
And the temperature measuring hole structures are arranged at the upper end and the lower end of the crucible.
Through the technical scheme, the characteristic that the melting point of the tantalum carbide is higher than the sublimation temperature of the silicon carbide is utilized, and the tantalum carbide has chemical inertness to the growth of the silicon and hydrogen high-purity semi-insulating silicon carbide crystal at high temperature, so that the corrosion of silicon-rich gas to the inner wall of the tantalum structure is effectively avoided, the silicon carbide is prevented from being generated in the temperature measuring hole, a large number of nucleation points cannot be provided for the subsequent growth of the silicon carbide, and the blockage of the temperature measuring hole is avoided.
In the prior art, in the growth process of silicon carbide crystals, as the graphite crucible is of a pore structure, gas in the crucible can continuously overflow, wherein the silicon-rich atmosphere can corrode carbon materials outside the crucible and react with the carbon materials to generate silicon carbide, particularly at gas channels such as upper and lower temperature measuring holes, the generation of the silicon carbide is particularly rapid, the temperature measurement Kong Ji is easy to be blocked, the temperature control is invalid, and the high-quality growth of the crystals is further affected. In one embodiment of the present invention, the porosity of the second graphite is set to be smaller than the porosity of the first graphite. Compared with the prior art, the arrangement can reduce the number of the overall holes of the crucible, thereby reducing the overflow rate of gas in the crucible, greatly improving the corrosion resistance of the temperature measuring hole area and effectively avoiding the blockage of the temperature measuring hole.
In an alternative embodiment, the crucible cover 52 is threadably coupled to the crucible body 51; the crucible upper section 53 is in threaded connection with the crucible lower section 54. In this way, the detachable connection between the crucible cover 52 and the crucible body 51 can be realized.
Preferably, a first internal thread 52a is arranged at the joint of the crucible cover 52 and the crucible upper section 53; a first external thread 53a matched with the first internal thread 52a is arranged at the joint of the crucible upper section 53 and the crucible cover 52; a second internal thread 53b is arranged at the joint of the crucible upper section 53 and the crucible lower section 54; the joint of the crucible lower section 54 and the crucible upper section 53 is provided with a second external thread 54a adapted to the second internal thread 53 b. The component with low thermal expansion coefficient is an internal thread, the component with high thermal expansion coefficient is an external thread, so that the internal thread and the external thread can be tightly matched at a high temperature stage, the sealing effect is better, and the gas overflow is less.
In an alternative embodiment, the upper end portion of the crucible upper section 53 has a greater coefficient of thermal expansion than the lower end portion thereof. The thermal expansion coefficient of the crucible cover 52 is smaller than that of the upper end part of the crucible upper section 53; the lower crucible section 54 has a coefficient of thermal expansion greater than that of the lower end portion of the upper crucible section.
In an alternative embodiment, the first internal thread 52a and the second internal thread 53b have a lower coefficient of thermal expansion than the first external thread 53a and the second external thread 54a.
In addition, as shown in fig. 5, the crucible assembly further includes a heat insulating layer 70, and the heat insulating layer 70 is wrapped around the outer circumference of the crucible body 51. Optionally, the thermal insulation layer 70 is a soft felt. The insulating layer 70 serves to reduce the rate of heat dissipation from the crucible.
A fifth aspect of the present invention provides a method of preventing clogging of a temperature measuring hole, comprising using the crucible assembly such that gas sublimated from a raw material region is prevented from clogging in the temperature measuring hole 30 when preparing silicon carbide crystals.
Through the technical scheme, the characteristic that the melting point of the tantalum carbide is higher than the sublimation temperature of the silicon carbide is utilized, and the tantalum carbide has chemical inertness to the growth of the silicon and hydrogen high-purity semi-insulating silicon carbide crystal at high temperature, so that the corrosion of silicon-rich gas to the inner wall of the tantalum structure is effectively avoided, the silicon carbide is prevented from being generated in the temperature measuring hole, a large number of nucleation points cannot be provided for the subsequent growth of the silicon carbide, and the blockage of the temperature measuring hole is avoided.
A sixth aspect of the present invention provides a method for producing a silicon carbide crystal, comprising the crucible assembly, the method comprising:
loading a proper amount of silicon carbide powder in the accommodating cavity 60;
placing a seed crystal 20a on the lower end surface of the crucible cover 52;
the silicon carbide powder is heated to the sublimation temperature of silicon carbide while controlling the temperature near the seed crystal 20a to be lower than the sublimation temperature so that the silicon carbide gas is sublimated at the seed crystal to obtain a silicon carbide crystal.
Through the technical scheme, the temperature measuring holes can be prevented from being blocked, so that accurate temperature is obtained, accurate data basis is provided for preparing silicon carbide crystal, and the silicon carbide crystal with better quality is prepared.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the invention are not described in detail in order to avoid unnecessary repetition.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (6)
1. A crucible assembly, the crucible assembly comprising:
the crucible comprises a crucible body (51) and a crucible cover (52); wherein the crucible body (51) is made of first graphite, and the crucible body (51) comprises an upper crucible section (53) and a lower crucible section (54) which are detachably connected with each other; the crucible cover (52) is made of second graphite, is detachably connected with the crucible body (51) and forms a containing cavity (60) with the crucible body (51);
temperature measurement hole structure includes:
a second body (20);
a temperature measuring hole (30) penetrating the second body (20);
a tantalum structure (40) comprising a first body (10) and a tantalum carbide layer overlying the first body (10); wherein the first body (10) is made of tantalum and any one or more metals of hafnium, niobium, zirconium and tungsten; the tantalum structure (40) is arranged in the temperature measuring hole (30) and covers the inner wall of the temperature measuring hole (30);
the temperature measuring hole structures are arranged at the upper end and the lower end of the crucible;
the second graphite has a porosity less than the porosity of the first graphite;
the crucible cover (52) is in threaded connection with the crucible body (51); the crucible upper section (53) is in threaded connection with the crucible lower section (54);
a first internal thread (52 a) is arranged at the joint of the crucible cover (52) and the crucible upper section (53); a first external thread (53 a) matched with the first internal thread (52 a) is arranged at the joint of the crucible upper section (53) and the crucible cover (52); a second internal thread (53 b) is arranged at the joint of the crucible upper section (53) and the crucible lower section (54); a second external thread (54 a) matched with the second internal thread (53 b) is arranged at the joint of the crucible lower section (54) and the crucible upper section (53); the first internal thread (52 a) and the second internal thread (53 b) have a lower coefficient of thermal expansion than the first external thread (53 a) and the second external thread (54 a).
2. The thermowell structure according to claim 1, characterized in that said second body (20) is a hard felt.
3. The crucible assembly of claim 1, wherein the crucible further comprises a heat insulating layer (70), the heat insulating layer (70) wrapping around the periphery of the crucible.
4. A crucible assembly according to claim 3, wherein the insulating layer (70) is a soft felt.
5. A method of preventing clogging of a temperature measuring hole, characterized in that the method comprises using the crucible assembly of any one of claims 1 to 4, so that gas sublimated from a raw material region is prevented from clogging in the temperature measuring hole (30) when preparing a silicon carbide crystal.
6. A method of producing a silicon carbide crystal comprising the crucible assembly of any one of claims 1 to 4, the method comprising:
loading a proper amount of silicon carbide powder into the accommodating cavity (60);
placing a seed crystal (20 a) on the lower end surface of the crucible cover (52);
the silicon carbide powder is heated to a sublimation temperature of silicon carbide while controlling a temperature in the vicinity of the seed crystal (20 a) to be lower than the sublimation temperature so that silicon carbide gas is sublimated at the seed crystal to obtain silicon carbide crystals.
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| CN103374749A (en) * | 2012-04-28 | 2013-10-30 | 上海硅酸盐研究所中试基地 | Temperature measurement structure suitable for growing SiC crystal system by PVT (physical vapor transportation) method |
| CN203096233U (en) * | 2013-01-14 | 2013-07-31 | 河北同光晶体有限公司 | Crucible structure for growth of silicon carbide crystal |
| CN105420813A (en) * | 2015-12-22 | 2016-03-23 | 中国电子科技集团公司第二研究所 | Doping-element-free high-purity semi-insulating silicon carbide crystal growing device |
| CN205711044U (en) * | 2016-06-14 | 2016-11-23 | 河北同光晶体有限公司 | A kind of thermal field structure avoiding the thermometer hole blocking of insulation center, top |
| JP6869077B2 (en) * | 2017-03-30 | 2021-05-12 | 昭和電工株式会社 | Method for manufacturing silicon carbide single crystal ingot |
| JP6881357B2 (en) * | 2018-03-08 | 2021-06-02 | 信越半導体株式会社 | Method for manufacturing silicon carbide single crystal |
| CN213172678U (en) * | 2020-08-20 | 2021-05-11 | 广州南砂晶圆半导体技术有限公司 | Crucible for growing large-size silicon carbide single crystal |
| CN113136622A (en) * | 2021-04-22 | 2021-07-20 | 中国电子科技集团公司第四十六研究所 | PVT method airflow-oriented silicon carbide single crystal growth device and using method |
| CN215050634U (en) * | 2021-06-08 | 2021-12-07 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | Graphite heater of new-type tantalum crucible carbonization |
| CN114059154A (en) * | 2021-11-17 | 2022-02-18 | 宁波合盛新材料有限公司 | Silicon carbide single crystal growth device and method |
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