CN114657632A - 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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- CN114657632A CN114657632A CN202210173332.4A CN202210173332A CN114657632A CN 114657632 A CN114657632 A CN 114657632A CN 202210173332 A CN202210173332 A CN 202210173332A CN 114657632 A CN114657632 A CN 114657632A
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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 21
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 74
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 61
- 239000013078 crystal Substances 0.000 claims abstract description 48
- 239000007789 gas Substances 0.000 claims abstract description 24
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910003468 tantalcarbide Inorganic materials 0.000 claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000009529 body temperature measurement Methods 0.000 claims abstract description 19
- 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
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 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
- 238000005245 sintering Methods 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
- 230000000149 penetrating effect Effects 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
- 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
- 238000002360 preparation method Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 10
- 229910052715 tantalum Inorganic materials 0.000 abstract description 7
- 230000007797 corrosion Effects 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- 239000003575 carbonaceous material Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000004321 preservation 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
- 238000005520 cutting process 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
- 230000005855 radiation Effects 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
- 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
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000005092 sublimation method Methods 0.000 description 1
- 150000003481 tantalum Chemical class 0.000 description 1
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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
- 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
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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
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/002—Controlling or regulating
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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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- Organic Chemistry (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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- 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, an anti-blocking method of a temperature measuring hole and a preparation method of a silicon carbide crystal. Wherein, 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; the temperature measuring hole structure is arranged at the upper end and the lower end of the crucible. Through above-mentioned technical scheme, utilize tantalum carbide melting point to be higher than this characteristic of sublimation temperature of carborundum, and the chemical inertness that tantalum carbide has to silicon and hydrogen under the high temperature, effectively avoided the corruption of rich silicon gas to tantalum system structure inner wall, hinder carborundum to generate in the temperature measurement hole, this just can not provide a large amount of nucleation points and supply the follow-up growing up of carborundum, has avoided the jam in temperature measurement hole.
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, an anti-blocking method of a temperature measuring hole and a preparation method of a silicon carbide crystal.
Background
A wide bandgap semiconductor material represented by silicon carbide (SiC) and gallium nitride (GaN) is a third generation wide bandgap semiconductor following silicon (Si) and 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 developed wide-band-gap semiconductor material 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 of the SiC can meet the new requirements of modern electronic technology on high temperature, high frequency, high power and radiation resistance, has wide application requirements in the fields of LED illumination, electric energy conversion, radar communication and the like, and is regarded as one of the most promising materials in the field of semiconductor materials.
At present, in the aspect of silicon carbide crystal growth, a high-temperature sublimation method of a seed crystal is mainly adopted, and the method is also called a physical vapor transport method (PVT). In the method for growing silicon carbide crystals by PVT (physical vapor transport) generally, a graphite crucible is used for loading seed crystals and silicon carbide raw materials, a carbon-based soft felt, a hard felt and other fibrous heat preservation layers are wrapped outside the graphite crucible, and temperature measuring 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 the silicon carbide crystal grows, the raw material is required to be heated to over 2200 ℃, and meanwhile, the seed crystal is controlled at a slightly lower temperature, so that the raw material is sublimated from the raw material area and is sublimated to a single crystal at the seed crystal. In the growth process of the silicon carbide crystal, because the graphite crucible is in a pore structure, gas in the crucible can continuously overflow, wherein the carbon material outside the crucible can be corroded by the silicon-rich atmosphere and reacts with the carbon material to generate silicon carbide, and particularly, the silicon carbide is generated rapidly at gas channels such as an upper temperature measuring hole and a lower temperature measuring hole, so that the temperature measuring holes are extremely easy to block, the temperature control is invalid, and the high-quality growth of the crystal is influenced.
Disclosure of Invention
The invention aims to overcome the defects of invalid temperature control and low crystal growth quality of the existing PVT (physical vapor transport) 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 including 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 chemical inertia of the tantalum carbide to silicon and hydrogen at high temperature can be effectively avoided, 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 the 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 producing a tantalum structure, including: burying the first body in carbon powder and carrying out high-temperature sintering treatment at 2400 ℃ or above, so that a tantalum carbide layer is formed on the outer surface of the first body.
Through 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 the temperature measuring hole formed in the graphite crucible for growing the silicon carbide crystal, 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 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, including:
a second body;
the temperature measuring hole penetrates through the second body;
the tantalum structure of claim 1 or the tantalum structure obtained by the production method of claim 2, which is provided in the temperature measuring hole so as to cover the inner wall of the temperature measuring hole.
Through above-mentioned technical scheme, when installing this tantalum system structure in the temperature measurement hole, utilize this characteristic of tantalum carbide melting point be higher than the sublimation temperature of carborundum, and the chemical inertia that tantalum carbide has silicon and hydrogen under the high temperature, effectively avoided the corruption of rich silicon gas to tantalum system structure inner wall, hinder carborundum to generate in the temperature measurement hole, this just can not provide a large amount of nucleation points and supply the follow-up growing up of carborundum, avoided the jam in temperature measurement hole.
Further, the second body is a stiff 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.
The temperature measuring hole structures are arranged at the upper end and the lower end of the crucible.
Through above-mentioned technical scheme, utilize tantalum carbide melting point to be higher than this characteristic of sublimation temperature of carborundum, and the chemical inertness that tantalum carbide has to silicon and hydrogen under the high temperature, effectively avoided the corruption of rich silicon gas to tantalum system structure inner wall, hinder carborundum to generate in the temperature measurement hole, this just can not provide a large amount of nucleation points and supply the follow-up growing up of carborundum, has avoided the jam in temperature measurement hole.
Further, the porosity of the second graphite is less than the porosity of the first graphite.
Further, the crucible cover is in threaded connection with the crucible body; the upper section of the crucible is in threaded connection with the lower section of the crucible.
Furthermore, a first internal thread is arranged at the joint of the crucible cover and the upper section of the crucible; a first external thread matched with the first internal thread is arranged at the joint of the upper section of the crucible and the crucible cover; a second internal thread is arranged at the joint of the upper section of the crucible and the lower section of the crucible; a second external thread matched with the second internal thread is arranged at the joint of the lower section of the crucible and the upper section of the crucible; the first internal thread and the second internal thread have a lower coefficient of thermal expansion than the first external thread and the second external thread.
Further, the crucible also comprises a heat insulation layer, and the heat insulation layer is wrapped on the periphery of the crucible.
Further, the heat-insulating layer is soft felt.
The fifth aspect of the invention provides a temperature measuring hole anti-blocking method, which comprises the step of preventing gas sublimated from a raw material area from being blocked in a temperature measuring hole when the crucible assembly is used for preparing the silicon carbide crystal.
Through above-mentioned technical scheme, utilize tantalum carbide melting point to be higher than this characteristic of sublimation temperature of carborundum, and the chemical inertness that tantalum carbide has to silicon and hydrogen under the high temperature, effectively avoided the corruption of rich silicon gas to tantalum system structure inner wall, hinder carborundum to generate in the temperature measurement hole, this just can not provide a large amount of nucleation points and supply the follow-up growing up of carborundum, has avoided the jam in temperature measurement hole.
The invention in a sixth aspect provides a method for preparing silicon carbide crystals, 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 the silicon carbide, and simultaneously controlling the temperature near the seed crystal to be lower than the sublimation temperature so that the silicon carbide gas is desublimated at the seed crystal to obtain the silicon carbide crystal.
According to the technical scheme, the temperature measuring hole can be prevented from being blocked, so that the accurate temperature can be obtained, accurate data basis is provided for the preparation of the silicon carbide crystal, and the silicon carbide crystal with higher quality can be prepared.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
FIG. 1 is a schematic structural view of one embodiment of a tantalum structure of the present invention;
FIG. 2 is a schematic structural view of an embodiment of a temperature measuring hole structure according to the present invention;
FIG. 3 is a schematic structural view of one embodiment of the crucible assembly of the present invention;
FIG. 4 is an exploded view of FIG. 3;
FIG. 5 is a schematic structural view of another embodiment of the crucible assembly of the present invention.
Description of the reference numerals
10 a first body; 20a second body; 30 temperature measuring holes; 40 a tantalum structure; 51 a crucible body; 52 crucible covers; 53, cutting the crucible upwards; 54 cutting the crucible downwards; 53a first external thread; 53b second internal thread; 54a second external thread; 60 an accommodating cavity; 70 an insulating layer.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
In the present invention, the use of the terms of orientation such as "upper and lower" in the case where no description is made to the contrary generally means the orientation in the assembled and used state. "inner and outer" refer to the inner and outer contours of the respective component itself.
A first aspect of the present invention provides a tantalum structure, as shown in fig. 1, including a first body 10 and a tantalum carbide layer (not shown) covering 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 (between 3730 ℃ and 3830 ℃) of the tantalum carbide is higher than the sublimation temperature of the silicon carbide is utilized, and the tantalum carbide has chemical inertness for 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 silicon-rich gas can be effectively prevented from corroding the tantalum structure, so that 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.
A second aspect of the present invention provides a method for producing a tantalum structure, including: the first body 10 is buried in carbon powder and is subjected to high-temperature sintering treatment of 2400 ℃ or higher, so that a tantalum carbide layer is formed on the outer surface of the first body 10. The first body 10 forms a tantalum carbide layer on the outer surface of the first body 10 after being sintered at a high temperature of 2400 ℃ or higher, and the melting point of the tantalum carbide is 3730-3830 ℃, which 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 for 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 silicon-rich gas to the inner wall of the tantalum structure can be effectively avoided, the silicon carbide is prevented from being formed in the temperature measuring hole, a large number of nucleation points are not provided for the subsequent growth of the silicon carbide, and therefore the blockage of the temperature measuring hole is avoided
A third aspect of the present invention provides a temperature measurement hole structure, as shown in fig. 2, including:
a second body 20;
the temperature measuring hole 30 penetrates through the second body 20;
the tantalum structure 40 is arranged in the temperature measuring hole 30 and covers the inner wall of the temperature measuring hole 30.
By the 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 silicon-rich gas to the inner wall of the tantalum structure can be effectively avoided, 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 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; 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, detachably connected to the crucible body 51, and forms a receiving chamber 60 with the crucible body 51.
And the temperature measuring hole structures 40 are arranged at the upper end and the lower end of the crucible respectively.
Through above-mentioned technical scheme, utilize this characteristic of tantalum carbide melting point be higher than the sublimation temperature of carborundum, and the chemical inertness that tantalum carbide has to the growth of high-purity semi-insulating carborundum crystal of silicon and hydrogen under the high temperature, effectively avoided the corruption of rich silicon gas to tantalum system structure inner wall, hinder carborundum to generate in the temperature measurement hole, this just can not provide a large amount of nucleation points and supply the subsequent growth of carborundum, avoided the jam in temperature measurement hole.
In the prior art, in the growth process of silicon carbide crystals, because a graphite crucible is in a pore structure, gas in the crucible can continuously overflow, wherein the carbon material outside the crucible can be corroded and reacts with the carbon material to generate silicon carbide in a silicon-rich atmosphere, and particularly, the silicon carbide is generated rapidly at gas channels such as upper and lower temperature measuring holes, so that the temperature measuring holes are extremely easy to block, the temperature control fails, and the high-quality growth of the crystals is further influenced. 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 total pore number 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 and the crucible lower section 54 are screwed together. Thus, the crucible cover 52 and the crucible body 51 can be detachably connected.
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 matched with the second internal thread 53 b. Wherein, the part that coefficient of thermal expansion is low is the internal thread, and the part that coefficient of thermal expansion is high is the external screw thread, and the internal and external screw thread cooperation can be tighter in the high temperature stage like this, and sealed effect is better, and gas spills over less.
In an alternative embodiment, the upper end portion of the upper crucible section 53 has a higher coefficient of thermal expansion than the lower end portion. The coefficient of thermal expansion of the crucible cover 52 is smaller than that of the upper end part of the crucible upper section 53; the lower section 54 has a coefficient of thermal expansion greater than that of the lower end portion of the upper section.
In an alternative embodiment, the coefficient of thermal expansion of the first internal thread 52a and the second internal thread 53b is lower than the coefficient of thermal expansion of the first external thread 53a and the second external thread 54 a.
In addition, as shown in fig. 5, the crucible assembly further includes an insulating layer 70, and the insulating layer 70 is wrapped around the outer circumference of the crucible body 10. Optionally, the insulation layer 70 is a soft felt. The insulating layer 70 functions to reduce the heat dissipation rate of the crucible.
The fifth aspect of the invention provides a temperature measuring hole anti-blocking method, which comprises the step of preventing gas sublimated from a raw material area from being blocked in the temperature measuring hole 30 when the silicon carbide crystal is prepared by using the crucible assembly.
Through above-mentioned technical scheme, utilize this characteristic of tantalum carbide melting point be higher than the sublimation temperature of carborundum, and the chemical inertness that tantalum carbide has to the growth of high-purity semi-insulating carborundum crystal of silicon and hydrogen under the high temperature, effectively avoided the corruption of rich silicon gas to tantalum system structure inner wall, hinder carborundum to generate in the temperature measurement hole, this just can not provide a large amount of nucleation points and supply the subsequent growth of carborundum, avoided the jam in temperature measurement hole.
A sixth aspect of the present invention provides a silicon carbide crystal production method including the crucible assembly, the silicon carbide crystal production method including:
loading a proper amount of silicon carbide powder into the accommodating cavity 60;
a seed crystal 20a is placed on the lower end face of the crucible cover 52;
the silicon carbide powder is heated to the sublimation temperature of the silicon carbide, and the temperature near the seed crystal 20a is controlled to be lower than the sublimation temperature, so that the silicon carbide gas is desublimated at the seed crystal to obtain the silicon carbide crystal.
According to the technical scheme, the temperature measuring hole can be prevented from being blocked, so that the accurate temperature can be obtained, accurate data basis is provided for the preparation of the silicon carbide crystal, and the silicon carbide crystal with higher quality can be prepared.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are all within the protection scope of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. The invention is not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (12)
1. A tantalum structure, characterized in that it comprises a first body (10) and a tantalum carbide layer overlying said first body (10); wherein the first body (10) is made of any one or more metals of hafnium, niobium, zirconium and tungsten.
2. A method of producing the tantalum-made structure of claim 1, comprising: burying a first body (10) in carbon powder and carrying out high-temperature sintering treatment at 2400 ℃ or higher so that a tantalum carbide layer is formed on the outer surface of the first body (10).
3. A temperature measurement hole structure, characterized in that, the temperature measurement hole structure includes:
a second body (20);
a temperature measuring hole (30) penetrating through the second body (20);
the tantalum structure (40) of claim 1 or the tantalum structure (40) obtained by the production method of claim 2, wherein the tantalum structure (40) is disposed in the temperature measurement hole (30) and covers the inner wall of the temperature measurement hole (30).
4. Temperature bore structure according to claim 3, characterized in that the second body (20) is a stiff felt.
5. A crucible assembly, comprising:
a crucible including a crucible body (51) and a crucible cover (52); 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 an accommodating cavity (60) with the crucible body (51).
A temperature measuring hole structure according to any one of claims 3 to 4, which is arranged at the upper and lower ends of the crucible.
6. The crucible assembly of claim 5, wherein the porosity of the second graphite is less than the porosity of the first graphite.
7. The crucible assembly of claim 5, wherein the crucible cover (52) is threaded to the crucible body (51); the crucible upper section (53) is in threaded connection with the crucible lower section (54).
8. The crucible assembly according to claim 7, characterized in that the junction of the crucible cover (52) and the crucible upper section (53) is provided with a first internal thread (52 a); 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); a second external thread (54a) matched with the second internal thread (53b) is arranged at the joint of the crucible lower section (54) and the crucible upper section (53); 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 (54 a).
9. The crucible assembly of claim 5, further comprising an insulating layer (70), the insulating layer (70) being wrapped around an outer periphery of the crucible.
10. The crucible assembly of claim 9, wherein the insulating layer (70) is a soft felt.
11. A temperature sensing well anti-plugging method, characterized in that it comprises using a crucible assembly according to any one of claims 5-10 to prevent the plugging of the temperature sensing well (30) with gases sublimed from the feedstock area during the production of silicon carbide crystals.
12. A method of producing a silicon carbide crystal comprising the crucible assembly of any one of claims 5-10, the method comprising:
loading a proper amount of silicon carbide powder into the accommodating cavity (60);
placing a seed crystal (20a) on the lower end face of the crucible cover (52);
the silicon carbide powder is heated to the sublimation temperature of the silicon carbide, and the temperature near the seed crystal (20a) is controlled to be lower than the sublimation temperature, so that the silicon carbide gas is sublimated at the seed crystal to obtain the silicon carbide crystal.
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