CN117488407A - Preparation method and preparation device of tantalum carbide coating - Google Patents
Preparation method and preparation device of tantalum carbide coating Download PDFInfo
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- CN117488407A CN117488407A CN202311427438.3A CN202311427438A CN117488407A CN 117488407 A CN117488407 A CN 117488407A CN 202311427438 A CN202311427438 A CN 202311427438A CN 117488407 A CN117488407 A CN 117488407A
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- tantalum
- powder
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- silicon
- heating
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- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910003468 tantalcarbide Inorganic materials 0.000 title claims abstract description 74
- 239000011248 coating agent Substances 0.000 title claims abstract description 66
- 238000000576 coating method Methods 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 140
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 126
- 238000010438 heat treatment Methods 0.000 claims abstract description 109
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 99
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000002994 raw material Substances 0.000 claims abstract description 59
- 238000005192 partition Methods 0.000 claims abstract description 57
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 56
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 51
- 229910021332 silicide Inorganic materials 0.000 claims abstract description 49
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims abstract description 49
- 230000008021 deposition Effects 0.000 claims abstract description 44
- 238000011049 filling Methods 0.000 claims abstract description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 62
- 239000010439 graphite Substances 0.000 claims description 62
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 61
- 238000000151 deposition Methods 0.000 claims description 43
- 238000000034 method Methods 0.000 claims description 27
- 230000006698 induction Effects 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- 230000007423 decrease Effects 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000010030 laminating Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 10
- 229930195733 hydrocarbon Natural products 0.000 abstract description 8
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 8
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 7
- 150000001345 alkine derivatives Chemical class 0.000 abstract description 7
- 238000004880 explosion Methods 0.000 abstract description 7
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 239000010703 silicon Substances 0.000 description 27
- 229910052710 silicon Inorganic materials 0.000 description 27
- 239000007788 liquid Substances 0.000 description 13
- 239000010410 layer Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000011247 coating layer Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000009413 insulation Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910001936 tantalum oxide Inorganic materials 0.000 description 2
- 150000000475 acetylene derivatives Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052754 neon Inorganic materials 0.000 description 1
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 238000006467 substitution reaction 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
- 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
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0635—Carbides
-
- 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
- C30B23/02—Epitaxial-layer growth
Landscapes
- 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)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention relates to the technical field of semiconductors, in particular to a preparation method and a preparation device of a tantalum carbide coating, wherein the preparation method of the tantalum carbide coating comprises the steps of filling tantalum powder and silicon powder in a raw material stacking area, and placing a workpiece to be plated in a deposition area and on a partition plate; and heating the silicon powder and the tantalum powder by using a heating mechanism to generate gaseous silicon carbide and gaseous tantalum silicide, and enabling the gaseous silicon carbide and the gaseous tantalum silicide to move to the surface of the workpiece to be plated through the through hole to react to generate a tantalum carbide coating. According to the preparation method of the tantalum carbide coating, hydrocarbon and alkyne substances are not needed, so that the explosion danger is not easy to occur under the heating condition, and the safety is improved.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a preparation method and a preparation device of a tantalum carbide coating.
Background
Silicon carbide is a typical representation of third generation semiconductor materials, and has the characteristics of wide band gap, high critical electric field, high thermal conductivity, high carrier saturation drift velocity, good chemical stability and the like, so that the silicon carbide is widely applied to the preparation of high-frequency, high-power, high-temperature, high-frequency corrosion-resistant and radiation-resistant semiconductor devices.
The related art method for preparing silicon carbide single crystal mainly includes a physical vapor transport method (also called a modified PVT growth method), a chemical vapor deposition method and a liquid phase method, wherein the most mature process is the physical vapor transport method, which mainly includes three steps: sublimation of SiC sources, transport of sublimates, and crystallization; specifically, in the PVT growth method, a polycrystalline SiC raw material is usually placed at the bottom of a crucible, a seed crystal is placed at the top of the crucible, the temperature inside the crucible is between 2000 and 2300 ℃, inert gas is filled in the reaction process, and the SiC gas is transported from the surface to the seed crystal for crystallization by utilizing the temperature gradient existing between the raw material and the seed crystal.
In the process of producing silicon carbide single crystals by a physical vapor transport method, the parts required to be used are usually graphite pieces, and the graphite pieces are easy to corrode; in order to solve the problem that the graphite piece is easy to corrode, the chemical vapor deposition principle is adopted in the related art, and a tantalum carbide coating is formed on the surface of the graphite piece; however, this approach requires the use of hydrocarbons and acetylenes, which present a high risk under high temperature conditions.
Disclosure of Invention
The invention aims to provide a preparation method and a preparation device of a tantalum carbide coating, which do not need hydrocarbon and alkyne substances, are not easy to generate explosion hazard under heating conditions, and improve safety.
Embodiments of the invention may be implemented as follows:
the invention provides a preparation method of a tantalum carbide coating, which comprises the following steps:
providing a preparation device of a tantalum carbide coating, wherein the preparation device comprises a crucible and a heating mechanism arranged outside the crucible; the crucible comprises a crucible body, a baffle plate and a graphite plate; the crucible body is provided with a chamber; the partition board is arranged in the cavity to divide the cavity into a raw material area and a deposition area, and a plurality of through holes for communicating the raw material area and the deposition area are formed in the partition board; the graphite plate is positioned at one end of the raw material area far away from the deposition area and is arranged on the bottom wall of the crucible body, and a raw material stacking area is formed between the graphite plate and the partition plate;
filling tantalum powder and silicon powder in a raw material stacking area, and placing a workpiece to be plated in a deposition area and on a partition plate;
and heating the silicon powder and the tantalum powder by using a heating mechanism to generate gaseous silicon carbide and gaseous tantalum silicide, and enabling the gaseous silicon carbide and the gaseous tantalum silicide to move to the surface of the workpiece to be plated through the through hole to react to generate a tantalum carbide coating.
In an alternative embodiment, the step of heating the silicon powder and tantalum powder comprises:
heating silicon powder and tantalum powder to a first preset temperature and keeping the first preset time;
heating the silicon powder and the tantalum powder to a second preset temperature and keeping the second preset time;
wherein the second preset temperature is greater than the first preset temperature; the first preset temperature is a temperature at which at least part of silicon powder is melted, and the melted silicon powder reacts with the graphite plate and the tantalum powder respectively to generate silicon carbide and tantalum silicide; the second preset temperature is a temperature at which the silicon powder, the generated silicon carbide and the generated tantalum silicide sublimate into gas.
In an alternative embodiment, the first preset temperature is 1350-1450 ℃; and/or the number of the groups of groups,
the second preset temperature is 2100-2300 ℃; and/or the number of the groups of groups,
the first preset time is 30-600min; and/or the number of the groups of groups,
the second preset time is 180-600min.
In an alternative embodiment, the step of heating the silicon powder and tantalum powder to a first predetermined temperature comprises: heating silicon powder and tantalum powder to a first preset temperature according to the heating power of 0.8-1.2 kw/h; and/or the number of the groups of groups,
and heating the silicon powder and the tantalum powder to a second preset temperature, wherein the step comprises the following steps of: and heating the silicon powder and the tantalum powder to a second preset temperature according to the heating power of 0.8-1.2 kw/h.
In an alternative embodiment, the step of heating the silicon powder and tantalum powder using a heating mechanism includes:
heating by using a radio frequency induction heating furnace or a resistance heating furnace, and enabling the pressure in the radio frequency induction heating furnace or the resistance heating furnace to be smaller than the pressure in the crucible by a vacuum pump vacuumizing mode and/or an inert gas filling mode.
In an alternative embodiment, the step of filling the raw material stacking region with tantalum powder and silicon powder comprises the steps of:
paving silicon powder on the graphite plate, and paving tantalum powder on the silicon powder; and/or the number of the groups of groups,
and mixing the silicon powder and the tantalum powder and paving the mixture on a graphite plate.
In an alternative embodiment, prior to the step of heating the silicon powder and tantalum powder, further comprising:
and paving silicon carbide powder on the partition plate, and enabling the silicon carbide powder and the workpiece to be plated to be distributed at intervals.
In an alternative embodiment, the weight ratio of tantalum powder to silicon powder is (4-10): (1-2.5); and/or the number of the groups of groups,
the mol ratio of the tantalum powder to the silicon carbide powder is (4.5-5.5): (2.5-3.5): (4.5-5.5); and/or the number of the groups of groups,
the thickness of the graphite plate is greater than or equal to 5mm.
In an alternative embodiment, the workpiece to be plated comprises a first end face and a second end face which are oppositely arranged, and a growth face connecting the first end face and the second end face;
placing a workpiece to be plated in a deposition area and on a partition plate, comprising:
and placing the workpiece to be plated in the deposition area and on the partition plate, attaching the first end face of the workpiece to be plated to the partition plate, and arranging the second end face of the workpiece to be plated away from the partition plate.
In alternative embodiments, the workpiece to be coated is an arc-shaped workpiece or a ring-shaped workpiece.
In an alternative embodiment, the method further comprises:
a seed plate is disposed at an end of the deposition zone remote from the feedstock zone so that gaseous silicon carbide generated during the step of heating the silicon powder and tantalum powder may also be moved to the seed plate to grow silicon carbide crystals.
In a second aspect, the invention also provides a preparation device of the tantalum carbide coating, which comprises a crucible and a heating mechanism arranged outside the crucible; the crucible comprises a crucible body, a baffle plate and a graphite plate; the crucible body is provided with a chamber; the partition board is arranged in the cavity to divide the cavity into a raw material area and a deposition area, and a plurality of through holes for communicating the raw material area and the deposition area are formed in the partition board; the graphite plate is positioned at one end of the raw material area far away from the deposition area and is arranged on the bottom wall of the crucible body, and a raw material stacking area is formed between the graphite plate and the partition plate; wherein,
the raw material stacking area is used for filling tantalum powder and silicon powder, and the partition board is used for placing the workpiece to be plated and enabling the workpiece to be plated to be located in the deposition area.
In an alternative embodiment, the crucible further comprises:
the annular coaming is located between baffle and the graphite slab, and one end is connected with the graphite slab, and the other end and baffle butt, and circumference lateral wall and the laminating of the circumference lateral wall of crucible body, graphite slab, baffle and annular coaming enclose and close and constitute the raw materials and stack the region.
In an alternative embodiment, the crucible further comprises:
the flow guiding piece is arranged at one end of the deposition area far away from the raw material area, the flow guiding piece is provided with a top end far away from the raw material area and a bottom end close to the raw material area, the top end of the flow guiding piece is attached to the top wall of the crucible body, the circumferential side wall of the flow guiding piece is attached to the circumferential inner wall of the crucible body, a flow guiding channel penetrating through the flow guiding piece is arranged in the flow guiding piece, the flow guiding channel extends from the top end of the flow guiding piece to the bottom end of the flow guiding piece, and the caliber of the flow guiding channel decreases from the bottom end of the flow guiding piece to the top end of the flow guiding piece;
the seed crystal plate is arranged at one end of the deposition area far away from the raw material area and is positioned in the diversion channel.
In an alternative embodiment, the method further comprises:
the workpiece to be plated comprises a first end face and a second end face which are oppositely arranged, and a growth face connecting the first end face and the second end face; the workpiece to be plated is arranged in the deposition area and on the partition board, the first end face of the workpiece to be plated is attached to the partition board, and the second end face of the workpiece to be plated is far away from the partition board.
In alternative embodiments, the workpiece to be coated is an arc-shaped workpiece or a ring-shaped workpiece.
The preparation method and the preparation device of the tantalum carbide coating provided by the embodiment of the invention have the beneficial effects that:
in the preparation method of the tantalum carbide coating provided by the embodiment of the invention, the used raw materials comprise the tantalum powder and the silicon powder, the tantalum powder and the silicon powder are filled in the raw material stacking area, when the silicon powder and the tantalum powder are heated, the silicon powder is melted to form silicon liquid, the silicon liquid can react with a graphite plate to generate silicon carbide, and the generated silicon carbide can form protection on the surface of the graphite plate so as to prevent the heated gaseous silicon from corroding the graphite plate, and can gasify the generated silicon carbide so as to provide a silicon carbide atmosphere for generating tantalum carbide through reaction, namely generate gaseous silicon carbide; meanwhile, the silicon liquid formed by melting the silicon powder can also react with the tantalum powder to generate tantalum silicide, the tantalum silicide is gasified under the heating condition to provide a tantalum silicide atmosphere for generating tantalum carbide by reaction, and the silicon can also form silicon atmosphere to move upwards and pass through the tantalum powder along with the heating so as to generate the tantalum silicide atmosphere, namely gaseous tantalum silicide; after the gaseous silicon carbide and the gaseous tantalum silicide pass through the partition plate, the gaseous silicon carbide and the gaseous tantalum silicide can move to the surface of a workpiece to be plated under the action of a radial temperature gradient of the crucible and react to generate a tantalum carbide coating. Therefore, the preparation method of the tantalum carbide coating does not need to use hydrocarbon and alkyne substances, and further the explosion danger is not easy to occur under the heating condition, so that the safety is improved.
The raw material stacking area of the tantalum carbide coating preparation device provided by the embodiment of the invention is used for filling tantalum powder and silicon powder, and the baffle is used for placing a workpiece to be plated and enabling the workpiece to be plated to be positioned in the deposition area; when the heating mechanism outside the crucible is used for heating, the tantalum powder and the silicon powder filled in the raw material stacking area can be heated to generate gaseous silicon carbide and gaseous tantalum silicide, and the gaseous silicon carbide and the gaseous tantalum silicide move to the surface of the workpiece to be plated through the through hole to react to generate the tantalum carbide coating. The tantalum carbide coating prepared by the preparation device is simple in mode, low in preparation cost, free of hydrocarbon and alkyne substances, and not prone to explosion hazard under heating conditions, and safety is improved.
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 cross-sectional view of a crucible in accordance with an embodiment of the present invention at a first view angle;
fig. 2 is a cross-sectional view of a crucible in accordance with an embodiment of the present invention at a second view angle.
Icon: 010-crucible; 100-crucible body; 200-a flow guide; 210-a seed plate; 310-graphite plates; 320-annular coaming; 330-a raw material stacking area; 400-separator; 500-a workpiece to be plated; 600-heat preservation felt.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the invention, as presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
In the description of the present invention, it should be noted that, if the terms "upper", "lower", "inner", "outer", and the like indicate an azimuth or a positional relationship based on the azimuth or the positional relationship shown in the drawings, or the azimuth or the positional relationship in which the inventive product is conventionally put in use, it is merely for convenience of describing the present invention and simplifying the description, and it is not indicated or implied that the apparatus or element referred to must have a specific azimuth, be configured and operated in a specific azimuth, and thus it should not be construed as limiting the present invention.
Furthermore, the terms "first," "second," and the like, if any, are used merely for distinguishing between descriptions and not for indicating or implying a relative importance.
It should be noted that the features of the embodiments of the present invention may be combined with each other without conflict.
Referring to fig. 1 and 2, the embodiment of the invention provides a method for preparing a tantalum carbide coating, which can utilize a preparation device of the tantalum carbide coating to generate the tantalum carbide coating on the surface of a workpiece to be coated, and can also generate the tantalum carbide coating on the surface of the workpiece to be coated and simultaneously grow silicon carbide crystals.
The preparation device of the tantalum carbide coating comprises a crucible 010 and a heating mechanism (not shown) arranged outside the crucible; the crucible 010 includes a crucible body 100, a baffle 400, and a graphite plate 310; the crucible body 100 has a chamber; the partition 400 is arranged in the cavity to divide the cavity into a raw material area and a deposition area, and a plurality of through holes for communicating the raw material area and the deposition area are formed in the partition 400; the graphite plate 310 is positioned at one end of the raw material area far away from the deposition area and is arranged on the bottom wall of the crucible body 100, and a raw material stacking area 330 is formed between the graphite plate 310 and the partition 400; wherein the raw material stacking region 330 is used for filling tantalum powder and silicon powder, and the partition 400 is used for placing the workpiece to be plated and positioning the workpiece to be plated in the deposition region. The tantalum carbide coating is prepared by using the preparation device of the tantalum carbide coating, the mode is simple, the preparation cost is low, hydrocarbon and alkyne substances are not needed, and further, the explosion danger is not easy to occur under the heating condition, and the safety is improved.
Optionally, separator 400 is a porous graphite sheet. Optionally, the heating mechanism is a radio frequency induction heating furnace or a resistance heating furnace.
Optionally, the crucible 010 further includes an annular enclosure plate 320, where the annular enclosure plate 320 is located between the partition plate 400 and the graphite plate 310, one end is connected to the graphite plate 310, the other end is abutted to the partition plate 400, and the circumferential side wall is attached to the circumferential side wall of the crucible body 100, and the graphite plate 310, the partition plate 400, and the annular enclosure plate 320 enclose a raw material stacking area 330. By the arrangement, the annular coaming 320 and the graphite plate 310 can jointly form a box structure so as to conveniently contain tantalum powder and silicon powder.
The crucible 010 further comprises a flow guiding piece 200 and a seed crystal plate 210, wherein the flow guiding piece 200 is arranged at one end of the deposition area far away from the raw material area, the flow guiding piece 200 is provided with a top end far away from the raw material area and a bottom end close to the raw material area, the top end of the flow guiding piece 200 is attached to the top wall of the crucible body, the circumferential side wall of the flow guiding piece 200 is attached to the circumferential inner wall of the crucible body, a flow guiding channel penetrating through the flow guiding piece 200 is arranged in the flow guiding piece 200, the flow guiding channel extends from the top end of the flow guiding piece 200 to the bottom end of the flow guiding piece 200, and the caliber of the flow guiding channel decreases from the bottom end of the flow guiding piece 200 to the top end of the flow guiding piece 200; the seed plate 210 is disposed at an end of the deposition zone remote from the source zone and within the flow directing channel. The deflector 200 serves to guide the vaporized raw material toward a seed plate 210 provided at the top of the crucible 010. The flow guide 200 may be a graphite flow guide.
Optionally, the crucible 010 further includes a thermal insulation felt 600, and the thermal insulation felt 600 is disposed outside the crucible body 100, so as to maintain the reaction temperature by using the thermal insulation felt 600, and reduce the loss of temperature.
Optionally, the preparation device of the tantalum carbide coating further comprises a workpiece 500 to be plated, wherein the workpiece 500 to be plated comprises a first end face and a second end face which are oppositely arranged, and a growth face connecting the first end face and the second end face; the workpiece 500 to be plated is arranged in the deposition area and on the partition 400, a first end face of the workpiece 500 to be plated is attached to the partition 400, and a second end face of the workpiece 500 to be plated is far away from the partition 400. In this way, various gasified reaction materials can be more reliably moved to the growth surface of the workpiece 500 to be coated, and further, a tantalum carbide coating can be more reliably formed on the growth surface of the workpiece 500 to be coated.
Further, the workpiece 500 to be plated is an arc-shaped workpiece or a ring-shaped workpiece, and it may be a graphite workpiece.
The preparation method of the tantalum carbide coating provided by the embodiment of the invention comprises the following steps: filling tantalum powder and silicon powder in a raw material stacking area 330, and placing a workpiece 500 to be plated in a deposition area and on a baffle 400; the silicon powder and the tantalum powder are heated by a heating mechanism to generate gaseous silicon carbide and gaseous tantalum silicide, and the gaseous silicon carbide and the gaseous tantalum silicide pass through the through holes of the baffle 400 and move to the surface of the workpiece 500 to be plated to react under the action of a radial temperature gradient of the crucible 010 to generate a tantalum carbide coating.
In the preparation method of the tantalum carbide coating, when silicon powder and tantalum powder are heated, the silicon powder is melted to form silicon liquid, the silicon liquid can react with the graphite plate 310 to generate silicon carbide, and the generated silicon carbide can form protection on the surface of the graphite plate 310 to prevent gaseous silicon formed by heating from corroding the graphite plate 310, and can gasify the generated silicon carbide to provide a silicon carbide atmosphere for reacting to generate tantalum carbide, namely to generate gaseous silicon carbide (reaction formula: si+c=sic); at the same time, the silicon powder melt to form silicon liquid can also react with tantalum powder to form tantalum silicide (reaction formula: 5ta+3si=ta 5 Si 3 ) The tantalum silicide is gasified under heating conditions to provide a tantalum silicide atmosphere that reacts to form tantalum carbide, and as heating proceeds the silicon also forms a silicon atmosphere that moves upward and through the tantalum powder to form siliconA tantalum oxide atmosphere, i.e. forming gaseous tantalum silicide (equation: 5ta+3si=ta) 5 Si 3 ) The method comprises the steps of carrying out a first treatment on the surface of the After the gaseous silicon carbide and the gaseous tantalum silicide pass through the baffle 400, they can be moved to the surface of the workpiece 500 to be coated by the radial temperature gradient of the crucible 010 and reacted to form a tantalum carbide coating (reaction: ta 5 Si 3 +5sic=5tac+8si). Therefore, the preparation method of the tantalum carbide coating does not need to use hydrocarbon and alkyne substances, and further the explosion danger is not easy to occur under the heating condition, so that the safety is improved.
Specifically, since a large amount of gaseous substances (including gaseous tantalum silicide, gaseous silicon and gaseous silicon carbide) are generated in the raw material stacking region 330 under the partition 400, resulting in an increase in pressure in the raw material stacking region under the partition 400, each gaseous substance flows upward through the partition 400, and the gaseous tantalum silicide is also affected by the radial temperature gradient of the crucible body 100 during the ascent in the crucible body 100, moves in the radial direction of the crucible body 100 toward the center of the crucible body 100, so that tantalum silicide is slowly deposited on the workpiece 500 to be coated supported by the partition 400, i.e., a tantalum oxide layer of silicon is formed on the workpiece 500 to be coated; meanwhile, gaseous silicon carbide is also affected by the radial temperature gradient of the crucible body 100, flows along the radial direction of the crucible body 100 towards the center of the crucible body 100, and reacts with tantalum silicide on the workpiece 500 to be plated to generate tantalum carbide when flowing onto the workpiece 500 to be plated, so that the purpose of plating a tantalum carbide coating on the workpiece 500 to be plated can be achieved.
Wherein, the radial temperature of the crucible body 100 is expressed as: the temperature of both sides of the crucible body 100 is higher than the temperature of the central region of the crucible body 100.
In addition, the preparation method of the embodiment of the invention generates the tantalum carbide coating on the surface of the workpiece 500 to be coated by the reaction of the tantalum silicide and the silicon carbide which are moved to the surface of the workpiece 500 to be coated, and the process of generating the tantalum carbide coating is not limited by the volume and the shape of the workpiece 500 to be coated and the size of the crucible body 100, so that the method has better universality and can be used for coating the workpiece 500 to be coated with the tantalum carbide coating with various sizes, particularly large sizes; when the size of the crucible body 100 is large enough, a plurality of workpieces 500 to be coated can be coated with tantalum carbide coating at the same time, which is beneficial to reducing the cost.
The manner in which the tantalum powder and the silicon powder are filled in the raw material stacking region 330 may be selected as desired; in the embodiment of the invention, silicon powder is paved on the graphite plate 310, and then tantalum powder is paved on the silicon powder. In this way, when the silicon powder is melted to form silicon liquid, the silicon liquid can be ensured to react with the graphite plate 310 reliably to generate silicon carbide, so that on one hand, the silicon carbide is ensured to further reliably protect the graphite plate 310, and on the other hand, the formation of a silicon carbide atmosphere is ensured; furthermore, the silicon powder is laid under the tantalum powder, and the silicon powder is vaporized and moved upward in the crucible body 100 during heating, and passes through the tantalum powder to etch the tantalum powder, that is, to react the silicon with the tantalum to form tantalum silicide (Ta 5 Si 3 The reaction formula: 5ta+3si=ta 5 Si 3 ) The formation of a tantalum silicide atmosphere is ensured.
Of course, in other embodiments, silicon powder and tantalum powder may be mixed and then laid on the graphite plate 310.
The weight ratio of tantalum powder to silicon powder can be selected according to the needs, for example: the weight ratio of the tantalum powder to the silicon powder is (4-10): (1-2.5), specifically, the weight ratio of tantalum powder to silicon powder may be 4:1, 4:1.5, 4:2.5, 5:1, 5:2, 5:2.5, 6:1, 6:1.5, 6:2.5, 7:1, 7:2, 7:2.5, 8:1, 8:1.5, 8:2.5, 9:1, 9:1.5, 9:2.5, 10:1, 10:1.5, 10:2.5, etc.
In the embodiment of the invention, before the step of heating the silicon powder and the tantalum powder, the method further comprises the following steps: the silicon carbide powder is laid on the spacer 400 and is spaced apart from the workpiece 500 to be plated, i.e., the silicon carbide powder is not in contact with the workpiece 500 to be plated placed on the spacer 400. In this way, a silicon carbide atmosphere can be provided using silicon carbide powder directly deposited on the spacer 400, ensuring that the tantalum carbide coating is reliably deposited on the surface of the workpiece 500 to be coated.
Silicon carbide powder is paved on the baffle 400, and the amounts of tantalum powder, silicon powder and silicon carbide powder are as follows: the molar ratio is (4.5-5.5): (2.5-3.5): (4.5-5.5), for example: 5:3:5, 4.5:2.5:4.5, 5.5:3.5:5.5, 5:2.5:5.5, 5.5:3:4.5, etc.
The thickness of the graphite sheet may be greater than or equal to 5mm; wherein, when the silicon carbide powder is not additionally laid on the separator 400, the thickness of the graphite sheet is 5-10mm, for example: 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, etc.; when silicon carbide powder is additionally laid on the separator 400, the thickness of the graphite sheet is 5mm or more.
In the preparation method of the tantalum carbide coating, the steps of heating silicon powder and tantalum powder specifically comprise the following steps: heating silicon powder and tantalum powder to a first preset temperature and keeping the first preset time; heating the silicon powder and the tantalum powder to a second preset temperature and keeping the second preset time; wherein the second preset temperature is greater than the first preset temperature; the first preset temperature is a temperature at which at least part of silicon powder is melted, and the melted silicon powder reacts with the graphite plate and the tantalum powder respectively to generate silicon carbide and tantalum silicide; the second preset temperature is a temperature at which the silicon powder, the generated silicon carbide and the generated tantalum silicide sublimate into gas. In the initial stage of heating, heating is carried out at a first preset temperature which is relatively low, so that when silicon powder is melted, the tantalum powder can be ensured to still exist in a solid form, the silicon liquid can reliably react with the tantalum powder to generate tantalum silicide, and the tantalum silicide can be gasified into tantalum silicide atmosphere at a second preset temperature which is higher in subsequent temperature; meanwhile, under the second preset temperature condition, silicon is enabled to be gasified to form an upward moving silicon atmosphere, the silicon atmosphere can penetrate through the tantalum powder, the tantalum powder is etched and reacted, and a tantalum silicide atmosphere is generated; in this way, a sufficient tantalum silicide atmosphere is ensured.
Optionally, the first preset temperature is 1350-1450 ℃, for example: 1350 ℃, 1370 ℃, 1400 ℃, 1420 ℃, 1450 ℃, etc.; the first preset time is 30-600min, for example: 30min, 100min, 150min, 200min, 250min, 300min, 350min, 400min, 450min, 500min, 550min, 600min, etc. Under the control of the temperature and the heating time, the silicon powder can be fully melted to form silicon liquid, and not only can a silicon carbide protective layer be reliably generated by utilizing the silicon liquid and the graphite plate 310 so as to be attached to the surface of the graphite plate 310, so that the gasified silicon is prevented from corroding the graphite plate 310; and the tantalum powder can be ensured to be stably kept in a solid state, so that the solid tantalum powder can be ensured to reliably react with silicon liquid to generate tantalum silicide, and preparation is made for providing a tantalum silicide atmosphere subsequently.
Optionally, in the step of heating the silicon powder and the tantalum powder to the first preset temperature: using an intermediate frequency induction heating furnace, the heating power is 0.8-1.2kw/h, for example: silicon powder and tantalum powder are heated to a first preset temperature of 0.8kw/h, 0.9kw/h, 1.0kw/h, 1.1kw/h, 1.2kw/h, etc.
Optionally, the second preset temperature is 2100-2300 ℃, for example: 2100 ℃, 2150 ℃, 2200 ℃, 2250 ℃, 2300 ℃, etc.; the second preset time is 180-600min, for example: 180min, 200min, 250min, 300min, 350min, 400min, 450min, 500min, 550min, 600min, etc. Continuing to heat at a relatively high temperature, and sublimating the tantalum silicide generated in the earlier stage to form a tantalum silicide atmosphere along with the extension of time; moreover, due to the increase in temperature, a large amount of silicon atmosphere is formed to move upward and pass through the tantalum powder to etch tantalum that has not reacted with the silicon liquid and directly form a tantalum silicide atmosphere, not only ensuring the amount of tantalum silicide atmosphere but also ensuring the efficiency of generating the tantalum silicide atmosphere.
It should be noted that, by controlling the time for which the second preset temperature is maintained, the thickness of the tantalum carbide coating layer on the workpiece 500 to be coated can be controlled, that is, when the time for which the tantalum carbide coating layer is maintained at the second preset temperature is longer, the thickness of the tantalum carbide coating layer is formed thicker, whereas the time for which the tantalum carbide coating layer is maintained at the second preset temperature is shorter, and the thickness of the tantalum carbide coating layer is formed thinner.
Optionally, in the step of heating the silicon powder and the tantalum powder to the second preset temperature, an intermediate frequency induction heating furnace is used, wherein the heating power is 0.8-1.2kw/h, for example: 0.8kw/h, 0.9kw/h, 1.0kw/h, 1.1kw/h, 1.2kw/h, etc., and then heating the silicon powder and tantalum powder from the first preset temperature to the second preset temperature.
In the embodiment of the invention, an intermediate frequency induction heating furnace is used for heating, and the intermediate frequency induction heating furnace is used for vacuumizing through a vacuum pump of the intermediate frequency induction heating furnace, and inert gas is introduced into the intermediate frequency induction heating furnace to enable the pressure in the furnace to be smaller than the pressure in a crucible; in this way, the pressure in the furnace is in a negative pressure state relative to the pressure in the crucible, and the pressure in the crucible is in a positive pressure state relative to the pressure in the furnace, so that the silicon carbide atmosphere can be deposited on the seed crystal rapidly.
Alternatively, the furnace pressure is less than the crucible pressure and the absolute value of the pressure difference is 0.1-20mbar (e.g. 0.1mbar, 1mbar, 2mbar, 5mbar, 10mbar, 12mbar, 15mbar, 18mbar, 20mbar, etc.), or 1-100mbar (e.g. 1mbar, 10mbar, 20mbar, 30mbar, 40mbar, 50mbar, 60mbar, 70mbar, 80mbar, 90mbar, 100mbar, etc.). When the pressure in the furnace is less than the pressure in the crucible and the difference is 0.1-20mbar or 1-100mbar, the state of the pressure in the furnace may be referred to as a micro negative pressure state, and the state of the pressure in the crucible may be referred to as a micro positive pressure state, in which the silicon carbide atmosphere in the crucible is facilitated to be deposited on the seed crystal more rapidly.
Alternatively, the pressure in the furnace may be 1-990mbar, for example: 1mbar, 100mbar, 200mbar, 300mbar, 500mbar, 600mbar, 700mbar, 900mbar, 990mbar and the like, and the pressure in the furnace is less than the pressure in the crucible.
Of course, in other embodiments, the pressure in the intermediate frequency induction heating furnace is controlled to be smaller than the pressure in the crucible, and the intermediate frequency induction heating furnace can be vacuumized or inert gas can be introduced into the intermediate frequency induction heating furnace.
It should be noted that, the air pressure in the intermediate frequency induction heating furnace may refer to: the outside of the crucible body 100 sealing the pressure inside the quartz tube of the crucible body 100, the pressure inside the furnace being less than the pressure inside the crucible may mean that the pressure inside the quartz tube is less than the pressure inside the crucible.
The inert gas includes, but is not limited to, helium (He), neon (Ne), or argon (Ar).
In the embodiment of the invention, while tantalum powder and silicon powder are heated so that gaseous silicon carbide and gaseous tantalum silicide pass through the baffle 400 to move to a deposition area above the baffle 400, so that a tantalum carbide coating is formed on the surface of a workpiece 500 to be plated, the gaseous silicon carbide can also move to the seed crystal plate 210 positioned at the top of the crucible body 100 under the action of an axial temperature gradient in the crucible body 100, so as to grow into silicon carbide crystals. In this way, the preparation method of the tantalum carbide coating not only can plate a layer of tantalum carbide coating on the surface of the workpiece 500 to be plated so as to form a protective layer on the surface of the workpiece 500 to be plated, but also can prepare crystals at the same time, thereby improving the utilization rate of raw materials and reducing the cost.
The present invention will be described in detail by way of specific examples.
Example 1
Paving a layer of silicon powder on the graphite plate, and paving a layer of tantalum powder above the silicon powder; the partition plate is disposed in the chamber of the crucible such that the chamber of the crucible is divided into a raw material region and a deposition region.
Placing a workpiece to be plated in a deposition area and on a partition plate; and paving silicon carbide powder on the partition board, and enabling the silicon carbide powder on the partition board not to contact with the workpiece to be plated. The molar ratio of the Ta powder to the silicon powder to the SiC powder is 5:3:5.
Controlling the pressure in the medium-frequency induction heating furnace to be 20mbar; heating the silicon powder and the tantalum powder to 1400 ℃ according to the heating power of 1kw/h, and keeping for 30min; and heating to 2200 ℃ continuously according to the heating power of 1kw/h, and keeping for 180min.
Example 2
Paving a layer of silicon powder on the graphite plate, and paving a layer of tantalum powder above the silicon powder; the partition plate is disposed in the chamber of the crucible such that the chamber of the crucible is divided into a raw material region and a deposition region. The weight ratio of the Ta powder to the silicon powder is 4:1.
And placing the workpiece to be plated on the partition board.
Controlling the furnace pressure of the medium-frequency induction heating furnace to be 0.1mbar; heating the silicon powder and the tantalum powder to 1450 ℃ according to the heating power of 1.2kw/h, and keeping for 600min; and then heating to 2300 ℃ continuously according to the heating power of 1.2kw/h, and keeping for 600min.
Example 3
Paving a layer of silicon powder on the graphite plate, and paving a layer of tantalum powder above the silicon powder; the partition plate is disposed in the chamber of the crucible such that the chamber of the crucible is divided into a raw material region and a deposition region. The weight ratio of the Ta powder to the silicon powder is 10:1.5.
And placing the workpiece to be plated on the partition board.
Controlling the pressure in the medium-frequency induction heating furnace to be 10mbar; heating the silicon powder and the tantalum powder to 1350 ℃ according to the heating power of 0.8kw/h, and keeping for 100min; heating to 2200 deg.C at heating power of 0.8kw/h, and maintaining for 400min.
Example 4
Paving a layer of silicon powder on the graphite plate, and paving a layer of tantalum powder above the silicon powder; the partition plate is disposed in the chamber of the crucible such that the chamber of the crucible is divided into a raw material region and a deposition region. The weight ratio of the Ta powder to the silicon powder is 8:2.5.
And placing the workpiece to be plated on the partition board.
Controlling the pressure in the medium-frequency induction heating furnace to be 12mbar; heating the silicon powder and the tantalum powder to 1420 ℃ according to the heating power of 1.1kw/h, and keeping for 300min; and then heating to 2250 ℃ continuously according to the heating power of 1kw/h, and maintaining for 350min.
In summary, according to the preparation method of the tantalum carbide coating, the tantalum carbide coating is generated on the surface of the workpiece to be plated by utilizing the generated tantalum silicide atmosphere and silicon carbide atmosphere, so that hydrocarbon and alkyne substances are not needed, further, the explosion danger is not easy to occur under the heating condition, and the safety is improved; the efficiency of the plating layer can be improved, and the cost of the plating layer can be reduced; at the same time, crystals can also be grown during coating.
The present invention is not limited to the above embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (16)
1. A method of producing a tantalum carbide coating, comprising:
providing a preparation device of a tantalum carbide coating, wherein the preparation device comprises a crucible and a heating mechanism arranged outside the crucible; the crucible comprises a crucible body, a baffle plate and a graphite plate; the crucible body is provided with a cavity; the partition board is arranged in the cavity to divide the cavity into a raw material area and a deposition area, and a plurality of through holes which are communicated with the raw material area and the deposition area are formed in the partition board; the graphite plate is positioned at one end of the raw material area, which is far away from the deposition area, and is arranged on the bottom wall of the crucible body, and a raw material stacking area is formed between the graphite plate and the partition plate;
filling tantalum powder and silicon powder in the raw material stacking area, and placing a workpiece to be plated in the deposition area and on the partition plate;
and heating the silicon powder and the tantalum powder by using the heating mechanism to generate gaseous silicon carbide and gaseous tantalum silicide, and enabling the gaseous silicon carbide and the gaseous tantalum silicide to move to the surface of the workpiece to be plated through the through hole to react to generate a tantalum carbide coating.
2. The method of producing a tantalum carbide coating as claimed in claim 1, wherein said step of heating said silicon powder and said tantalum powder comprises:
heating the silicon powder and the tantalum powder to a first preset temperature and keeping the first preset time;
heating the silicon powder and the tantalum powder to a second preset temperature and keeping the second preset time;
wherein the second preset temperature is greater than the first preset temperature; the first preset temperature is a temperature at which at least part of the silicon powder is melted, and the melted silicon powder reacts with the graphite plate and the tantalum powder to generate silicon carbide and tantalum silicide respectively; the second preset temperature is a temperature at which the silicon powder, the generated silicon carbide and the generated tantalum silicide sublimate into gas.
3. The method of producing a tantalum carbide coating according to claim 2, wherein said first preset temperature is 1350-1450 ℃; and/or the number of the groups of groups,
the second preset temperature is 2100-2300 ℃; and/or the number of the groups of groups,
the first preset time is 30-600min; and/or the number of the groups of groups,
the second preset time is 180-600min.
4. A method of preparing a tantalum carbide coating according to claim 3, wherein said step of heating said silicon powder and said tantalum powder to a first predetermined temperature comprises: heating the silicon powder and the tantalum powder to a first preset temperature according to the heating power of 0.8-1.2 kw/h; and/or the number of the groups of groups,
the step of heating the silicon powder and the tantalum powder to a second preset temperature comprises the following steps: and heating the silicon powder and the tantalum powder to a second preset temperature according to the heating power of 0.8-1.2 kw/h.
5. The method of producing a tantalum carbide coating according to claim 1, wherein the step of heating said silicon powder and said tantalum powder using said heating mechanism comprises:
heating by using a radio frequency induction heating furnace or a resistance heating furnace, and enabling the pressure in the radio frequency induction heating furnace or the resistance heating furnace to be smaller than the pressure in the crucible by a vacuum pump vacuumizing mode and/or an inert gas filling mode.
6. The method of producing a tantalum carbide coating according to claim 1, wherein said step of filling said raw material stacking region with tantalum powder and silicon powder comprises:
paving silicon powder on the graphite plate, and paving tantalum powder on the silicon powder; and/or the number of the groups of groups,
and mixing the silicon powder and the tantalum powder and paving the mixture on the graphite plate.
7. The method of producing a tantalum carbide coating as claimed in claim 1, further comprising, prior to the step of heating the silicon powder and the tantalum powder:
and paving silicon carbide powder on the partition plate, and enabling the silicon carbide powder and the workpiece to be plated to be distributed at intervals.
8. The method of producing a tantalum carbide coating according to claim 6 or 7, wherein the weight ratio of said tantalum powder to said silicon powder is (4-10): (1-2.5); and/or the number of the groups of groups,
the mol ratio of the tantalum powder to the silicon carbide powder is (4.5-5.5): (2.5-3.5): (4.5-5.5); and/or the number of the groups of groups,
the thickness of the graphite plate is greater than or equal to 5mm.
9. The method of producing a tantalum carbide coating according to claim 1, wherein said workpiece to be plated comprises a first end face and a second end face disposed opposite to each other, and a growth face connecting said first end face and said second end face;
the placing of the workpiece to be plated in the deposition area and on the separator comprises:
and placing the workpiece to be plated in the deposition area and on the partition board, attaching the first end face of the workpiece to be plated to the partition board, and arranging the second end face of the workpiece to be plated away from the partition board.
10. The method for producing a tantalum carbide coating according to claim 9, wherein said workpiece to be plated is an arc-shaped workpiece or an annular workpiece.
11. The method of producing a tantalum carbide coating according to claim 1, further comprising:
a seed plate is disposed at an end of the deposition zone remote from the feedstock zone such that the gaseous silicon carbide generated in the step of heating the silicon powder and the tantalum powder is also movable to the seed plate to grow into silicon carbide crystals.
12. The preparation device of the tantalum carbide coating is characterized by comprising a crucible and a heating mechanism arranged outside the crucible; the crucible comprises a crucible body, a baffle plate and a graphite plate; the crucible body is provided with a cavity; the partition board is arranged in the cavity to divide the cavity into a raw material area and a deposition area, and a plurality of through holes which are communicated with the raw material area and the deposition area are formed in the partition board; the graphite plate is positioned at one end of the raw material area, which is far away from the deposition area, and is arranged on the bottom wall of the crucible body, and a raw material stacking area is formed between the graphite plate and the partition plate; wherein,
the raw material stacking area is used for filling tantalum powder and silicon powder, and the partition board is used for placing a workpiece to be plated and enabling the workpiece to be plated to be located in the deposition area.
13. The apparatus for producing a tantalum carbide coating as claimed in claim 12, wherein the crucible further comprises:
the annular coaming is located the baffle with between the graphite plate, one end with the graphite plate is connected, the other end with the baffle butt, and circumference lateral wall with the laminating of the circumference lateral wall of crucible body, the graphite plate the baffle with the annular coaming encloses to close and constitutes the raw materials is stacked the region.
14. The apparatus for producing a tantalum carbide coating as claimed in claim 12, wherein the crucible further comprises:
the flow guiding piece is arranged at one end of the deposition area, which is far away from the raw material area, the flow guiding piece is provided with a top end, which is far away from the raw material area, and a bottom end, which is close to the raw material area, the top end of the flow guiding piece is attached to the top wall of the crucible body, the circumferential side wall of the flow guiding piece is attached to the circumferential inner wall of the crucible body, a flow guiding channel penetrating through the flow guiding piece is arranged in the flow guiding piece, the flow guiding channel extends from the top end of the flow guiding piece to the bottom end of the flow guiding piece, and the caliber of the flow guiding channel decreases from the bottom end of the flow guiding piece to the top end of the flow guiding piece;
the seed crystal plate is arranged at one end of the deposition area far away from the raw material area and is positioned in the diversion channel.
15. The apparatus for producing a tantalum carbide coating as claimed in claim 12, further comprising:
the workpiece to be plated comprises a first end face and a second end face which are oppositely arranged, and a growth face connecting the first end face and the second end face; the workpiece to be plated is arranged in the deposition area and on the partition board, a first end face of the workpiece to be plated is attached to the partition board, and a second end face of the workpiece to be plated is far away from the partition board.
16. The apparatus for producing a tantalum carbide coating according to claim 15, wherein said workpiece to be plated is an arc-shaped workpiece or an annular workpiece.
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