CN115595659A - Surface coating of graphite matrix, preparation method and application - Google Patents
Surface coating of graphite matrix, preparation method and application Download PDFInfo
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- CN115595659A CN115595659A CN202211364779.6A CN202211364779A CN115595659A CN 115595659 A CN115595659 A CN 115595659A CN 202211364779 A CN202211364779 A CN 202211364779A CN 115595659 A CN115595659 A CN 115595659A
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/183—Epitaxial-layer growth characterised by the substrate being provided with a buffer layer, e.g. a lattice matching layer
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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
- C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
- C30B25/02—Epitaxial-layer growth
- C30B25/18—Epitaxial-layer growth characterised by the substrate
- C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
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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
Abstract
The invention relates to the technical field of semiconductor epitaxial growth, and discloses a surface coating of a graphite substrate, a preparation method and application thereof, wherein the preparation method comprises the following steps: a transition layer and a single phase layer; transition layer and graphite base member take place the carbonization reaction and generate tantalum carbide, and the transition layer is high with graphite base member's degree of combination, is provided with a plurality of holes on the transition layer, and during these holes will be embedded in the single phase layer, form the gomphosis structure with the transition layer, promoted the cohesion of coating, solved among the prior art tantalum carbide coating and graphite base member degree of combination low easy drop lead to the life-span short, the not high problem of practicality.
Description
Technical Field
The invention relates to the technical field of semiconductor epitaxial growth, in particular to a surface coating of a graphite substrate, a preparation method and application thereof.
Background
In the third generation of semiconductor SiC and GaN production processes, existing coated graphite parts (SiC, BN coatings) chemically react with corrosive gases such as hydrogen and ammonia at high temperatures, which results in exposure of the graphite material to the production process; impurities in the graphite material and corrosive gases damage the graphite material, which can adversely affect crystal growth.
Tantalum carbide (TaC) is a transition metal carbide, has the advantages of high melting point, high hardness, good chemical stability, strong electric and heat conductivity and the like, can keep good mechanical performance in an ultra-high temperature environment (more than 3000 ℃), has the melting point of 3880 ℃, and has the advantages of high specific strength, good oxidation resistance and ablation resistance and the like; the advantages can ensure that the TaC coating still keeps a stable state in a harsh semiconductor environment, and is a coating with great application prospect.
However, because of the large difference of the thermal expansion coefficients between the tantalum carbide coating and the graphite substrate, the surface of the coating is easy to generate gaps, so that the bonding degree of the coating and the graphite substrate is low, the coating is easy to fall off, and the problems of short service life and low practicability are caused.
Disclosure of Invention
The invention aims to provide a surface coating of a graphite matrix, a preparation method and application thereof, and aims to solve the problems of short service life and low practicability caused by low bonding degree of a tantalum carbide coating and the graphite matrix and easy falling in the prior art.
The present invention is achieved in a first aspect, and provides a surface coating of a graphite substrate, which is coated on a surface of the graphite substrate, and includes:
a transition layer and a single phase layer;
the transition layer is arranged on the surface of the graphite substrate, holes arranged in an array are arranged on the transition layer, the single-phase layer is arranged on the transition layer, and the single-phase layer is embedded into the holes;
the transition layer is made of tantalum, tantalum and carbon mixture or tantalum, carbon and tantalum carbide mixture;
the single-phase layer is made of tantalum carbide.
In one embodiment, the voids occupy between 10% and 30% of the area of the transition layer.
In one embodiment, the transition layer has a thickness of between 1-10 μm.
In one embodiment, the thickness of the single phase layer is between 20-35 μm.
In a second aspect, the present invention provides a graphite component having a surface coating, comprising: a graphite substrate, and a surface coating of any one of the graphite substrates provided in the first aspect;
the surface coating is arranged to coat the graphite substrate;
the graphite matrix has a thermal expansion coefficient of 5 × 10 -6 - 8×10 -6 between/K;
the density of the graphite matrix is 1.7-1.9 g/cm 3 ；
The graphite matrix has a total ash content of less than 100 ppm.
In a third aspect, the present invention provides a method for preparing a surface coating of a graphite substrate, for preparing the surface coating of any one of the graphite substrates provided in the first aspect, comprising:
s1: pretreating a graphite matrix;
s2: preparing a transition layer on the graphite substrate;
s3: punching the transition layer; the punching process comprises laser punching and ultrasonic punching;
s4: preparing a single-phase layer on the transition layer; the preparation method of the transition layer comprises chemical vapor deposition, slurry sintering and plasma spraying.
In one embodiment, the S1 includes:
s11: transferring the graphite substrate into a CVD reaction chamber;
s12: evacuating the CVD reaction chamber to a vacuum; the air pressure of the vacuum is between 1 and 100 Pa;
s13: delivering high-temperature hydrogen to the CVD reaction chamber, and enabling the hydrogen to carry out heat treatment on the graphite substrate; the temperature of the hydrogen is between 1000 and 1500 ℃, and the time of the heat treatment is between 1 and 3 hours.
In one embodiment, the S2 includes:
s21: transferring the graphite substrate to a CVD reaction chamber;
s22: delivering the mixed gas to the CVD reaction chamber through a carrier gas; the carrier gas is argon, and the mixed gas comprises penta-chlorinated methane, methane and hydrogen;
s23: and heating the CVD reaction chamber to 800-1300 ℃, and preserving the heat for 0.5-3 h.
In one embodiment, the S4 includes:
s41: transferring the graphite substrate to a CVD reaction chamber;
s42: delivering a gas mixture to the CVD reaction chamber by a carrier gas; the carrier gas is argon, and the mixed gas comprises penta-chlorinated methane, methane and hydrogen;
s43: and heating the CVD reaction chamber to 1800-2400 ℃, and preserving the heat for 1-10 h.
In one embodiment, the flow rate of the argon is 1-10L/min, the flow rate of the methane is 0.5-5L/min, and the flow rate of the hydrogen is 1-5L/min.
The invention provides a surface coating of a graphite matrix, a preparation method and application thereof, and has the following beneficial effects:
transition layer and graphite base member take place the carbonization reaction and generate tantalum carbide, and the transition layer is high with graphite base member's degree of combination, is provided with a plurality of holes on the transition layer, and during these holes will be embedded in the single phase layer, form the gomphosis structure with the transition layer, promoted the cohesion of coating, solved among the prior art tantalum carbide coating and graphite base member degree of combination low easy drop lead to the life-span short, the not high problem of practicality.
Drawings
FIG. 1 is a schematic structural diagram of a surface coating of a graphite substrate according to an embodiment of the present invention;
FIG. 2 is an X-ray diffraction pattern of a surface coating of a graphite substrate provided by an embodiment of the present invention;
FIG. 3 is a schematic step diagram of a method for preparing a surface coating of a graphite substrate according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of the step S1 of a method for preparing a surface coating of a graphite substrate according to an embodiment of the present invention;
FIG. 5 is a schematic diagram of the step S2 of the method for preparing the surface coating of the graphite substrate according to the embodiment of the present invention;
fig. 6 is a schematic step diagram of S4 of a method for preparing a surface coating of a graphite substrate according to an embodiment of the present invention.
Reference numerals are as follows: 1-transition layer, 2-single phase layer, 11-holes and 3-graphite matrix.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The same or similar reference numerals in the drawings of the present embodiment correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", etc. based on the orientation or positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but it is not intended to indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes and are not to be construed as limiting the present patent, and the specific meaning of the terms may be understood by those skilled in the art according to specific circumstances.
The following detailed description of implementations of the invention refers to specific embodiments.
Referring to FIG. 1, a preferred embodiment of the present invention is provided.
In a first aspect, the present invention provides a surface coating of a graphite substrate 3, coated on the surface of the graphite substrate 3, comprising:
a transition layer 1 and a single phase layer 2.
Specifically, the transition layer 1 is arranged on the surface of the graphite substrate 3, and the single-phase layer 2 is arranged on the transition layer 1; wherein, the thickness of the transition layer 1 is between 1 and 10 μm, and the thickness of the single-phase layer 2 is between 20 and 35 μm.
The transition layer 1 is made of tantalum, a mixture of tantalum and carbon, or a mixture of tantalum, carbon and tantalum carbide, it should be noted that tantalum and carbon may generate a carbonization reaction at a high temperature to generate tantalum carbide, and the graphite substrate 3 is made of carbon, so that when the transition layer 1 is disposed on the surface of the graphite substrate 3, referring to fig. 2, the transition layer 1 and the graphite substrate 3 contact each other to generate tantalum carbide, and thus the transition layer 1 and the graphite substrate 3 have a high bonding strength and a low thermal stress.
It should be noted that the thermal stress is a stress generated by an object not being able to expand and contract freely due to external constraint and mutual constraint between internal parts when the temperature changes, the conventional graphite surface coating has high thermal stress and low stability under high temperature conditions, while the transition layer 1 provided by the present invention has low thermal stress and thus has higher stability under high temperature conditions.
It will be appreciated that the transition layer 1 will assume a non-smooth condition and that this form of transition layer 1 will bond to a greater extent, since tantalum carbide will form at the site where the transition layer 1 and the graphite substrate 3 are released.
More specifically, the transition layer 1 is provided with regular and uniform holes 11, and the holes 11 can further reduce thermal stress; more specifically, single-phase layer 2's material is tantalum carbide, and consequently when setting up single-phase layer 2, single-phase layer 2 can fill hole 11 to realize transition layer 1 and single-phase layer 2's gomphosis, promoted transition layer 1 and single-phase layer 2's cohesion, make the coating have higher intensity.
Preferably, the holes 11 occupy between 10% and 30% of the area of the transition layer 1.
More preferably, the holes 11 occupy 20% of the area of the transition layer 1.
It should be noted that the hole 11 is not a single hole 11, but a plurality of uniform holes 11, and the holes 11 are uniformly distributed on the transition layer 1.
The invention provides a surface coating of a graphite matrix 3, which has the following beneficial effects:
transition layer 1 takes place carbonization reaction with graphite base member 3 and generates tantalum carbide, and transition layer 1 is high with graphite base member 3's combination degree, is provided with a plurality of holes 11 on transition layer 1, and the monophase layer will imbed in these holes 11, forms the gomphosis structure with transition layer 1, has promoted the cohesion of coating, has solved among the prior art tantalum carbide coating and graphite base member 3 combination degree low easy drop lead to the life-span short, the not high problem of practicality.
In a second aspect, the present invention provides a graphite component having a surface coating, comprising: a graphite substrate 3, and a surface coating of any one of the graphite substrates 3 as provided in the first aspect.
Specifically, the surface coating is disposed to cover the graphite substrate 3, that is, the surface coating is disposed on the outer side of the graphite substrate 3.
More specifically, the graphite base body 3 has a thermal expansion coefficient of 5X 10 -6 - 8×10 -6 The density of the graphite matrix 3 is between 1.7 and 1.9 g/cm 3， The total ash content of the graphite matrix 3 is less than 100 ppm.
The thermal expansion coefficient refers to a coefficient of regularity that geometric characteristics of a substance change with temperature change under the effect of expansion with heat and contraction with cold, and in most cases, the coefficient is a positive value. That is to say a temperature increase and volume enlargement; it is understood that the surface coating is provided on the surface of the graphite base body 3 in a high temperature environment, and therefore the thermal expansion coefficient of the graphite base material needs to be controlled within a predetermined range to prevent it from being excessively expanded to lose its performance in the high temperature environment in which the surface coating is provided.
The total ash is the weight percentage of the residual inorganic matter in the material before combustion after the material is combusted at a high temperature; it is understood that the surface coating is provided on the surface of the graphite base body 3 under a high temperature environment, and therefore the total ash content of the graphite base material needs to be controlled within a predetermined range to avoid the excessive loss of quality of the graphite base body 3 under the high temperature environment in which the surface coating is provided, which results in the failure of the graphite base body 3 to maintain the shape.
The invention provides a graphite component with a surface coating, which has the following beneficial effects:
transition layer 1 takes place carbonization reaction with graphite base member 3 and generates tantalum carbide, and transition layer 1 is high with graphite base member 3's combination degree, is provided with a plurality of holes 11 on transition layer 1, and the monophase layer will imbed in these holes 11, forms the gomphosis structure with transition layer 1, has promoted the cohesion of coating, has solved among the prior art tantalum carbide coating and graphite base member 3 combination degree low easy drop lead to the life-span short, the not high problem of practicality.
Referring to fig. 3, in a third aspect, the present invention provides a method for preparing a surface coating of a graphite substrate 3, for preparing the surface coating of any one of the graphite substrates 3 provided in the first aspect, comprising:
s1: the graphite matrix 3 is pretreated.
S2: a transition layer 1 is prepared on a graphite substrate 3.
S3: the transition layer 1 is perforated.
S4: a single-phase layer 2 is prepared on the transition layer 1.
The invention provides a preparation method of a surface coating of a graphite matrix 3, which has the following beneficial effects:
transition layer 1 and graphite base member 3 take place the carbonization reaction and generate tantalum carbide, and transition layer 1 is high with graphite base member 3's degree of combination, is provided with a plurality of holes 11 on transition layer 1, and among these holes 11, 2 monophase layers will imbed, forms the gomphosis structure with transition layer 1, has promoted the cohesion of coating, has solved among the prior art tantalum carbide coating and graphite base member 3 degree of combination low easy drop lead to the life-span short, the not high problem of practicality.
Specifically, referring to fig. 4, S1 includes:
s11: the graphite substrate 3 is transferred into a CVD reactor chamber.
S12: vacuumizing the CVD reaction chamber; the pressure of the vacuum is between 1 Pa and 100 Pa.
S13: high-temperature hydrogen is conveyed to the CVD reaction chamber, and the graphite matrix 3 is subjected to heat treatment by the hydrogen; the temperature of the hydrogen is between 1000 and 1500 ℃, and the time of the heat treatment is between 1 and 3 hours.
The CVD reaction chamber is a reaction chamber for performing a CVD reaction, and the CVD reaction is a chemical vapor deposition reaction in which a gaseous or vapor substance reacts on a gas-phase or gas-solid interface to form a solid deposit.
It should be noted that the metal heat treatment is a process of placing a metal workpiece in a certain medium, heating to a proper temperature, keeping the temperature for a certain time, cooling in different media at different speeds, and controlling the performance of the metal workpiece by changing the microstructure of the surface or the interior of the metal material.
It is understood that, since the graphite substrate 3 is heat-treated with hydrogen in the embodiment provided by the present invention, the CVD reaction chamber needs to be evacuated first to avoid the interference of the remaining gases with the thermal reaction.
Specifically, referring to fig. 5, S2 includes:
s21: the graphite substrate 3 was transferred to a CVD reaction chamber.
S22: conveying the mixed gas to the CVD reaction chamber through a carrier gas; the carrier gas is argon, and the mixed gas comprises penta-chlorinated methane, methane and hydrogen.
S23: heating the CVD reaction chamber to 800-1300 ℃, and preserving the temperature for 0.5-3 h.
It will be appreciated that the purpose of the carrier gas is to carry the mixture into the CVD chamber and therefore the carrier gas needs to be an inert gas which does not itself react, in the embodiment provided herein the carrier gas is argon.
It should be noted that the material of the transition layer 1 is any one of (1) pure tantalum, (2) tantalum and carbon mixture, and (3) tantalum, carbon, and tantalum carbide mixture, so in order to fabricate the transition layer 1, tantalum element and carbon element need to be provided, and in the embodiment provided by the present invention, the mixed gas includes tantalum pentachloride (TaCl) 5 ) Methane (CH) 4 ) And hydrogen (H) 2 ) Wherein, the tantalum element is derived from tantalum pentachloride, and the carbon element is derived from methane.
More specifically, the molar ratio of tantalum element to carbon element in the mixed gas is 1.2-2: 5.
specifically, referring to fig. 6, S4 includes:
s41: the graphite substrate 3 was transferred to a CVD reaction chamber.
S42: conveying the mixed gas to the CVD reaction chamber through a carrier gas; the carrier gas is argon, and the mixed gas comprises penta-chlorinated methane, methane and hydrogen.
S43: heating the CVD reaction chamber to 1800-24000 ℃, and preserving the heat for 1-10 h.
It will be appreciated that S4 corresponds to S2, the carrier gas is argon and the mixed gas comprises penta-chlorinated methanes and hydrogen.
Wherein, the tantalum pentachloride is solid at normal temperature, and needs to be heated to 160-300 ℃ to be gaseous.
More specifically, the molar ratio of tantalum element to carbon element in the mixed gas is 10-15 μm.
In some embodiments, the flow rate of argon is 1-10L/min, the flow rate of methane is 0.5-5L/min, and the flow rate of hydrogen is 1-5L/min.
In some embodiments, the method of preparing the transition layer 1 includes chemical vapor deposition, slurry sintering, and plasma spraying.
The preparation method used in the invention for S21-S23 is chemical vapor deposition; in addition, the slurry sintering method is to convert the powder material into a compact body on the surface of the graphite matrix 3 through sintering so as to obtain a surface coating; plasma spraying is a technology for strengthening and modifying the surface of a material, and can ensure that the surface of a matrix has the performances of wear resistance, corrosion resistance, high-temperature oxidation resistance, electric insulation, heat insulation, radiation protection, wear reduction, sealing and the like.
It is to be understood that the present invention is not limited to the process used to produce the transition layer 1, i.e., suitable processes other than chemical vapor deposition, slurry sintering, and plasma spraying can also be used to produce the transition layer 1 in the present invention.
In some embodiments, the process used for drilling in S3 includes laser drilling and ultrasonic drilling.
Specifically, laser drilling is to irradiate the material to be processed with a high-power-density laser beam, so that the material is heated to a vaporization temperature quickly and is vaporized to form the holes 11.
More specifically, the energy of the laser is more than 40J, the pulse width is 300 fs-1 ps, the flow of protective gas at the laser scanning speed is 4-5L/min, and the drilling depth is 10-15 μm.
Specifically, ultrasonic drilling is a special machining process in which a tool is vibrated at a small amplitude by using an ultrasonic frequency, and the surface of a workpiece material is gradually crushed by hammering the workpiece surface with an abrasive free in a liquid between the tool and the workpiece.
It is to be understood that the invention is not limited to the process used for drilling, i.e., suitable processes other than laser drilling and ultrasonic drilling can be used for drilling in the invention.
The following are examples provided by the present invention:
example 1:
s1: a6-inch graphite disk was used as the graphite substrate 3, which was placed in a CVD reaction chamber, the CVD reaction chamber was evacuated, and then hydrogen gas was supplied into the CVD reaction chamber at a flow rate of 10L/min, and the graphite disk was baked at a high temperature of 1100 ℃ for 2 hours in a hydrogen gas atmosphere. Wherein the graphite has a thermal expansion coefficient of 5.5 × 10 -6 K, bulk density 1.85 g/cm -3 The total ash content was 10 ppm.
S2: inputting a mixed gas of tantalum pentachloride, methane and hydrogen into a CVD reaction chamber by taking argon as a carrier gas, raising the temperature of the reaction chamber to 1100 ℃, and preserving the temperature for 1h to react to generate a transition layer 1 with the thickness of 5 mu m; wherein the flow rate of argon is 10L/min, the flow rate of methane is 2L/min, the tantalum pentachloride is stored in a gasification tank, the temperature is 200 ℃, and the pressure in the tank is 10w Pa.
S3: the transition layer 1 is perforated by laser perforation, and the area of the holes 11 occupies 20% of the area of the transition layer 1.
S4: argon is used as carrier gas, mixed gas of tantalum pentachloride, methane and hydrogen is input into a CVD reaction chamber, the temperature of the reaction chamber is raised to 2400 ℃, and the temperature is kept for 10 hours to generate a single-phase layer 2 with the thickness of 30 mu m through reaction; wherein the flow rate of argon is 5L/min, the flow rate of methane is 2L/min, the flow rate of hydrogen is 1L/min, the tantalum pentachloride is stored in a gasification tank, the temperature of the tantalum pentachloride is 200 ℃, and the pressure in the tank is 10w Pa.
Example 2:
the graphite substrate of example 1 was replaced with a graphite substrate having a bulk density of 1.85 g/cm3 and a coefficient of thermal expansion of 6.8X 10-6/k, and the remaining steps were identical to those of example 1.
Example 3:
the temperature of the vaporizer used to store tantalum pentachloride of example 1 was set to 160 c and the remaining steps were in accordance with example 1.
Example 4:
the temperature of the vaporizer used to store tantalum pentachloride of example 1 was set to 220 c and the remaining steps were in accordance with example 1.
Example 5:
the flow rate of the carrier gas in example 1 was changed to 5L/min, and the remaining steps were identical to those in example 1.
Example 6:
the flow rate of the carrier gas in example 1 was changed to 10L/min, and the remaining steps were identical to those in example 1.
Example 7:
the hydrogen flow rate in S4 in example 1 was changed to 0L/min, and the rest of the procedure was identical to that in example 1.
Example 8:
the reaction temperature of S4 in example 1 was adjusted to 1800 ℃ and the rest of the procedure was in accordance with example 1.
Example 9:
the reaction time for S4 in example 1 was adjusted to 6h, and the rest of the procedure was in accordance with example 1.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A surface coating of a graphite substrate, which is coated on the surface of the graphite substrate, is characterized by comprising:
a transition layer and a single phase layer;
the transition layer is arranged on the surface of the graphite substrate, holes arranged in an array are arranged on the transition layer, the single-phase layer is arranged on the transition layer, and the single-phase layer is embedded into the holes;
the transition layer is made of tantalum, tantalum and carbon mixture or tantalum, carbon and tantalum carbide mixture;
the single-phase layer is made of tantalum carbide.
2. The coating on the surface of the graphite substrate according to claim 1, wherein the area of the pores occupies 10% to 30% of the surface area of the transition layer.
3. A coating on the surface of a graphite substrate according to claim 1, wherein the thickness of the transition layer is between 1 and 10 μm and the thickness of the single-phase layer is between 20 and 35 μm.
4. A graphite component having a surface coating, comprising: a graphite substrate, and a surface coating of any one of the graphite substrates of claims 1-4;
the surface coating is arranged to coat the graphite substrate;
the graphite matrix has a thermal expansion coefficient of 5 × 10 -6 - 8×10 -6 between/K;
the density of the graphite matrix is 1.7-1.9 g/cm 3 ；
The graphite matrix has a total ash content of less than 100 ppm.
5. A method for preparing a surface coating of a graphite substrate, for preparing a surface coating of a graphite substrate according to any one of claims 1 to 4, comprising:
s1: pretreating a graphite matrix;
s2: preparing a transition layer on the graphite substrate;
s3: punching the transition layer; the punching process comprises laser punching and ultrasonic punching;
s4: preparing a single-phase layer on the transition layer; the preparation method of the transition layer comprises chemical vapor deposition, slurry sintering and plasma spraying.
6. The method of claim 6, wherein S1 comprises:
s11: transferring the graphite substrate into a CVD reaction chamber;
s12: evacuating the CVD reaction chamber to a vacuum; the air pressure of the vacuum is between 1 Pa and 100 Pa;
s13: delivering high-temperature hydrogen to the CVD reaction chamber, and enabling the hydrogen to carry out heat treatment on the graphite substrate; the temperature of the hydrogen is between 1000 and 1500 ℃, and the time of the heat treatment is between 1 and 3 hours.
7. The method of claim 6, wherein the step S2 comprises:
s21: transferring the graphite substrate to a CVD reaction chamber;
s22: delivering a gas mixture to the CVD reaction chamber by a carrier gas; the carrier gas is argon, and the mixed gas comprises penta-chlorinated methane, methane and hydrogen;
s23: and heating the CVD reaction chamber to 800-1300 ℃, and preserving the heat for 0.5-3 h.
8. The method of claim 6, wherein the step S4 comprises:
s41: transferring the graphite substrate to a CVD reaction chamber;
s42: delivering a gas mixture to the CVD reaction chamber by a carrier gas; the carrier gas is argon, and the mixed gas comprises penta-chlorinated methane, methane and hydrogen;
s43: and heating the CVD reaction chamber to 1800-2400 ℃, and preserving the heat for 1-10 h.
9. The method of claim 8 or claim 9, wherein the flow rate of argon is 1-10L/min, the flow rate of methane is 0.5-5L/min, and the flow rate of hydrogen is 1-5L/min.
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| CN116813383A (en) * | 2023-07-14 | 2023-09-29 | 中电化合物半导体有限公司 | Tantalum carbide coating and preparation method thereof |
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| US20120040172A1 (en) * | 2005-02-14 | 2012-02-16 | Hirokazu Fujiwara | Tantalum Carbide-Coated Carbon Material and Production Method Thereof |
| CN106431498A (en) * | 2016-09-05 | 2017-02-22 | 江苏协鑫特种材料科技有限公司 | Graphite/silicon carbide compact composite material preparation method |
| CN114807891A (en) * | 2022-06-14 | 2022-07-29 | 安徽钽盾科技有限公司 | Preparation method of graphite-based high-temperature-resistant corrosion-resistant thermal field material with TaC coating deposited on surface |
| CN114956825A (en) * | 2022-06-14 | 2022-08-30 | 安徽钽盾科技有限公司 | Method for growing TaC coating on surface of graphite-based material |
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| US20120040172A1 (en) * | 2005-02-14 | 2012-02-16 | Hirokazu Fujiwara | Tantalum Carbide-Coated Carbon Material and Production Method Thereof |
| CN106431498A (en) * | 2016-09-05 | 2017-02-22 | 江苏协鑫特种材料科技有限公司 | Graphite/silicon carbide compact composite material preparation method |
| CN114807891A (en) * | 2022-06-14 | 2022-07-29 | 安徽钽盾科技有限公司 | Preparation method of graphite-based high-temperature-resistant corrosion-resistant thermal field material with TaC coating deposited on surface |
| CN114956825A (en) * | 2022-06-14 | 2022-08-30 | 安徽钽盾科技有限公司 | Method for growing TaC coating on surface of graphite-based material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116813383A (en) * | 2023-07-14 | 2023-09-29 | 中电化合物半导体有限公司 | Tantalum carbide coating and preparation method thereof |
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