CN117026140A - Compact ceramic coating, preparation method thereof and chemical vapor deposition equipment - Google Patents
Compact ceramic coating, preparation method thereof and chemical vapor deposition equipment Download PDFInfo
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- CN117026140A CN117026140A CN202311005617.8A CN202311005617A CN117026140A CN 117026140 A CN117026140 A CN 117026140A CN 202311005617 A CN202311005617 A CN 202311005617A CN 117026140 A CN117026140 A CN 117026140A
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- 238000005524 ceramic coating Methods 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 22
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 238000011068 loading method Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000005240 physical vapour deposition Methods 0.000 claims description 3
- 238000007751 thermal spraying Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 230000000052 comparative effect Effects 0.000 description 14
- 230000007797 corrosion Effects 0.000 description 10
- 238000005260 corrosion Methods 0.000 description 10
- 239000011248 coating agent Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 230000006378 damage Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 150000004767 nitrides Chemical class 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005324 grain boundary diffusion Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 238000002679 ablation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000009528 severe injury Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
Classifications
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- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/18—After-treatment
-
- 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
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4404—Coatings or surface treatment on the inside of the reaction chamber or on parts thereof
-
- 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
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/56—After-treatment
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
- C23C18/1208—Oxides, e.g. ceramics
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
-
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1295—Process of deposition of the inorganic material with after-treatment of the deposited inorganic material
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C4/11—Oxides
-
- 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
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/134—Plasma spraying
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Ceramic Engineering (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention provides a compact ceramic coating, a preparation method thereof and chemical vapor deposition equipment, and belongs to the technical field of ceramic coatings. The preparation method of the compact ceramic coating comprises the following steps: (1) Preparing a prefabricated ceramic coating on the surface of a workpiece, and marking the obtained workpiece with the prefabricated ceramic coating on the surface as a prefabricated workpiece; (2) And loading the prefabricated workpiece into a die, and performing pulse current sintering under the action of axial pressure to obtain a workpiece with the surface provided with the compact ceramic coating, which is recorded as a finished workpiece. The invention firstly adopts a conventional preparation method to prepare the prefabricated ceramic coating, and then under the combined action of an external load and a pulse current, the surface tension, creep dislocation and extremely high temperature gradient after microscopic local melting are generated in the prefabricated ceramic coating, so that the initial grain boundary of the prefabricated ceramic coating is gradually diffused, and finally the compact ceramic coating is formed.
Description
Technical Field
The invention belongs to the technical field of ceramic coatings, and particularly relates to a compact ceramic coating, a preparation method thereof and chemical vapor deposition equipment.
Background
Chemical Vapor Deposition (CVD) techniques are widely used in the preparation of semiconductor materials, with various types of vapor phase reactions and various characteristics. During the deposition reaction, each component in the whole process chamber may be eroded by the reaction gas. In the long-term use process, the reliability of the process and the equipment cannot be guaranteed. Various attempts have been made to coat the inner cavity of the CVD equipment at home and abroad, and the traditional technology includes alumina, silicon carbide and the like, while the newer technology adopts aluminum fluoride, boron nitride and the like as the coating.
Oxide/carbide/fluoride/nitride ceramic coatings are inherently the presently preferred protective material for CVD equipment cavities, but in actual production, the ability of these ceramic coatings to prevent atmospheric attack is found by the skilled artisan to be largely determined by the pore size and number of the ceramic coatings. The oxide/carbide/fluoride/nitride ceramic coating prepared by the conventional method has the problem of larger porosity, so that the ceramic coating has lower capability of preventing atmosphere corrosion, and lower corrosion resistance of workpieces and product durability.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the related art to some extent. Therefore, the embodiment of the invention provides a compact ceramic coating, a preparation method thereof and chemical vapor deposition equipment, wherein the preparation method of the compact ceramic coating can greatly reduce the porosity of the ceramic coating and enable the ceramic coating to be in a non-porous form, so that the capability of preventing atmosphere corrosion of the ceramic coating is greatly improved, and the corrosion resistance of a workpiece and the durability of a product are greatly improved.
The embodiment of the invention provides a preparation method of a compact ceramic coating, which comprises the following steps:
(1) Preparing a prefabricated ceramic coating on the surface of a workpiece, and marking the obtained workpiece with the prefabricated ceramic coating on the surface as a prefabricated workpiece;
(2) And loading the prefabricated workpiece into a die, and performing pulse current sintering under the action of axial pressure to obtain a workpiece with the surface provided with the compact ceramic coating, which is recorded as a finished workpiece.
The preparation method provided by the embodiment of the invention has the following advantages and technical effects:
according to the embodiment of the invention, the prefabricated ceramic coating is prepared by adopting a conventional preparation method, and then under the combined action of an external load and a pulse current, the surface tension, creep dislocation and extremely high temperature gradient after microscopic local melting are generated in the prefabricated ceramic coating, so that the initial grain boundary of the prefabricated ceramic coating is gradually diffused, and finally the compact ceramic coating is formed.
In some embodiments, in step (1), the preformed ceramic coating is prepared using a thermal spray process, a sol gel process, a physical vapor deposition process, or a chemical vapor deposition process.
In some embodiments, the axial pressure in step (2) is 45-55MPa.
In some embodiments, in step (2), the local ramp rate is 500-1000 ℃/min.
In some embodiments, in step (2), the pulse width is 35-45ms and the pulse interval is 20-100ms.
In some embodiments, in step (2), the pulse width is 38-42ms and the pulse interval is 40-60ms.
In some embodiments, in step (2), the mold includes a hot-pressing mold having a cavity for accommodating the prefabricated workpiece and having an opening at an upper end and/or a lower end, and an upper pressing mold and a lower supporting mold disposed opposite to each other, the upper pressing mold and/or the lower supporting mold being slidable in the cavity of the hot-pressing mold, the upper pressing mold and/or the lower supporting mold being connected to a driving device, and the upper pressing mold and the lower supporting mold being connected to a pulse power source.
In addition, the embodiment of the invention also provides a compact ceramic coating, which is obtained by the preparation method of the embodiment of the invention.
The compact ceramic coating provided by the embodiment of the invention has the following advantages and technical effects:
compared with the prefabricated ceramic coating, the compact ceramic coating provided by the embodiment of the invention has lower porosity and tends to be in a nonporous form, so that the capability of preventing atmosphere corrosion of the ceramic coating is greatly improved, and the corrosion resistance of a workpiece and the durability of a product are greatly improved.
In addition, the embodiment of the invention also provides chemical vapor deposition equipment, and the inner wall of the process chamber of the chemical vapor deposition equipment is provided with the compact ceramic coating.
The chemical vapor deposition equipment provided by the embodiment of the invention has the following advantages and technical effects:
the process chamber of the chemical vapor deposition equipment provided by the embodiment of the invention has excellent corrosion resistance and greatly improves the durability.
Drawings
FIG. 1 is a schematic diagram of a mold used in a pulse current sintering process in a method of manufacturing an embodiment of the present invention;
fig. 2 is a schematic diagram of a pulse current sintering process in a method of making an embodiment of the present invention.
Reference numerals illustrate: 1-prefabricating a ceramic coating; 2-prefabricating a workpiece; 3-hot pressing a die; 31-cavity; 32-opening; 4-upper pressing die; 5-lower support die; 6-pulse power supply.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings. The embodiments described below by referring to the drawings are illustrative and intended to explain the present invention and should not be construed as limiting the invention.
The embodiment of the invention provides a preparation method of a compact ceramic coating, which comprises the following steps:
(1) Preparing a prefabricated ceramic coating 1 on the surface of a workpiece, and marking the obtained workpiece with the prefabricated ceramic coating 1 on the surface as a prefabricated workpiece 2;
(2) As shown in fig. 1 and 2, the prefabricated work piece 2 is put into a mold, and pulse current sintering is performed under the action of axial pressure, and the obtained work piece with the dense ceramic coating on the surface is denoted as a finished work piece.
Working principle: in the embodiment of the invention, any conventional preparation method can be adopted to prepare the prefabricated ceramic coating in the step (1), and the initial grain boundary diffusion of the prefabricated ceramic coating is promoted by using the external load and the surface tension of the local melt in the step (2), so that the power law creep of dislocation is improved; the pulse heating produces a short-time local temperature gradient, which also promotes the initial grain boundary diffusion of the prefabricated ceramic coating, and a compact ceramic coating is obtained. The gap of the prefabricated ceramic coating has larger contact resistance, and higher thermal power can be excited by pulse current, so that local melting is realized in a microscopic range, and the gap is filled with the locally melted coating by utilizing surface tension and external pressure, so that the dense ceramic coating of the embodiment of the invention is obtained, and a layer of the prefabricated ceramic coating is needed to carry out the step (2).
The direction corresponding to the diameter of the prefabricated work piece 2 is taken as a radial direction, and the direction perpendicular to the radial direction is taken as an axial direction, so the axial direction refers to the direction perpendicular to the prefabricated work piece 2 or the direction corresponding to the thickness of the prefabricated work piece 2.
The current or voltage pulses that occur repeatedly in cycles, called pulsed currents, occur either in the same direction or in alternating positive and negative directions. The pulse current obtained from the alternating current by rectification is also referred to as "pulsating direct current" and "pulsating direct voltage". Pulse current sintering, sometimes referred to as "spark sintering" or "plasma activated sintering," is a method of rapidly passing current through a sample to produce a ceramic coating. The sintering time of pulse current sintering is short, and the temperature rising is fast, thus being two advantages of preparing compact ceramic coating. The common current is continuous and uninterrupted, if the common electric heating is used for replacing the pulse current sintering in the step (2), the structure of the prefabricated ceramic coating can be damaged, the influence on the workpiece is larger, and the product performance is not improved. The embodiment of the invention adopts a pulse current sintering mode, only needs to melt nearby the gaps of the prefabricated ceramic coating, but does not have a heating area, and the temperature is generally not higher than 500 ℃. The local heating mode does not damage the workpiece and the prefabricated ceramic coating, and is beneficial to improving the product performance. When the unit cell integrity of the ceramic coating is improved, the contact resistance is greatly reduced, and local high temperature is not generated basically, so that the preparation of the compact ceramic coating is finished.
The ceramic coating which is the treatment object of the preparation method according to the embodiment of the present invention may be a ceramic coating such as oxide/carbide/fluoride/nitride. In any ceramic coating, the porosity of the obtained compact ceramic coating is obviously reduced and tends to be nonporous compared with that of a prefabricated ceramic coating after the preparation method of the embodiment of the invention.
The method for preparing the ceramic coating in step (1) is not particularly limited in the embodiment of the present invention, and any conventional method in the related art may be selected. For example, thermal spraying (flame, arc, plasma, etc.), sol-gel, physical vapor deposition or chemical vapor deposition, etc. may be used to prepare the preformed ceramic coating.
In some embodiments, the axial pressure in step (2) is 45-55MPa, e.g., 45MPa, 46MPa, 47MPa, 48MPa, 49MPa, 50MPa, 51MPa, 52MPa, 53MPa, 54MPa, 55MPa, etc. When the axial pressure is too small, the driving force is insufficient, so that pores are difficult to fill, and the compactness of the prepared coating cannot reach an ideal index. When the axial pressure is too high, the ceramic coating which has been prepared may be damaged, and may also cause mechanical damage to the workpiece to be coated due to the excessive stress.
In some embodiments, in step (2), the local heating rate is 500-1000 ℃/min, such as 500 ℃/min, 600 ℃/min, 700 ℃/min, 800 ℃/min, 900 ℃/min, 1000 ℃/min, and the like. The choice of the local heating rate is related to the melting point and the thermal conductivity of the ceramic coating, and in general, the higher the melting point is, the higher the thermal conductivity is, the faster the heating rate is required, and special cases exist. When the local heating rate is too low, local melting is difficult to achieve. When the local temperature rising speed is too high, the pulse current is too large, the compactness of the ceramic coating is not obviously improved any more, and the economical efficiency is reduced.
In some embodiments, in step (2), the pulse width is 35-45ms, e.g., 35ms, 36ms, 37ms, 38ms, 39ms, 40ms, 41ms, 42ms, 43ms, 44ms, 45ms, etc., and the pulse interval is 20-100ms, e.g., 20ms, 30ms, 40ms, 50ms, 60ms, 70ms, 80ms, 90ms, 100ms, etc. When the pulse width is too small or the pulse interval is too large, a sufficient temperature cannot be locally formed, and a micro-fused state at the aperture is generated. When the pulse width is too large or the pulse interval is too small, too much heat can damage the coating integrity and can also lead to damage to the workpiece. The current value of the pulse current is set according to the cross-sectional area of the workpiece. Preferably, in step (2), the pulse width is 38-42ms and the pulse interval is 40-60ms.
In some embodiments, in step (2), the pulse current sintering time is 1-20min, e.g., 1min, 3min, 6min, 8min, 10min, 12min, 14min, 16min, 18min, 20min, etc. When the pulse current sintering time is too short, the compactness of the ceramic coating is not improved. When the pulse current treatment time is too long, the integrity of the ceramic coating unit cell is improved, the contact resistance is greatly reduced, local high temperature is basically not generated any more, the densification effect cannot be further improved, and the economy is reduced.
In some embodiments, in step (2), as shown in fig. 1, the mold includes a hot press mold 3 and an upper press mold 4 and a lower support mold 5 disposed opposite to each other, the hot press mold 3 has a cavity 31 for accommodating the prefabricated workpiece 2, and the upper end and/or the lower end has an opening 32, the upper press mold 4 and/or the lower support mold 5 can slide in the cavity 2 of the hot press mold 3, the upper press mold 4 and/or the lower support mold 5 are connected to a driving device (not shown in the drawing), and the upper press mold 4 and the lower support mold 5 are connected to the pulse power source 6.
The upper pressing die 4 and the lower supporting die 5 are arranged as electrodes, a pulse power supply 6 is connected, and the direction of pulse current is consistent with the axial pressure. The pulse current and the axial pressure act simultaneously, the pulse current generates slight dissolution on the surface of the prefabricated ceramic coating, the area between the unit cells is melted, and meanwhile, the gap of the ceramic coating is filled by utilizing the external pressure and the capillary phenomenon, so that the structure of the prefabricated ceramic coating is not damaged, and the porosity of the obtained compact ceramic coating is greatly reduced relative to that of the prefabricated ceramic coating.
In addition, the embodiment of the invention also provides a compact ceramic coating, which is obtained by the preparation method of the embodiment of the invention.
Compared with the prefabricated ceramic coating, the compact ceramic coating provided by the embodiment of the invention has lower porosity and tends to be in a nonporous form, so that the capability of preventing atmosphere corrosion of the ceramic coating is greatly improved, and the corrosion resistance of a workpiece and the durability of a product are greatly improved.
In addition, the embodiment of the invention also provides chemical vapor deposition equipment, and the inner wall of the process chamber of the chemical vapor deposition equipment is provided with the compact ceramic coating.
The chemical vapor deposition equipment provided by the embodiment of the invention has the following advantages and technical effects:
the process chamber of the chemical vapor deposition equipment provided by the embodiment of the invention has excellent corrosion resistance and greatly improves the durability.
The present invention will be described in detail with reference to the following examples and drawings.
The structure of the mold used in the pulse current sintering process in the following examples and comparative examples is shown in fig. 1, the mold comprising a hot press mold 3 and upper and lower support molds 4 and 5 disposed opposite to each other up and down, the hot press mold 3 having a cavity 31 for accommodating the prefabricated work 2 and an opening 32 at an upper end, the upper press mold 4 being slidable in the cavity 2 of the hot press mold 3, the lower support mold 5 being held stationary, the upper press mold 4 being connected to a driving device (not shown in the drawing), the upper press mold 4 and the lower support mold 5 being connected to a pulse power source 6.
Example 1
A method for preparing a dense ceramic coating, comprising the steps of:
(1) Preparing a prefabricated alumina ceramic coating on the surface of a workpiece by adopting a plasma spraying method, wherein the average grain size of the prefabricated alumina ceramic coating is about 0.4 mu m, the porosity is 45%, and the obtained workpiece with the prefabricated alumina ceramic coating on the surface is recorded as a prefabricated workpiece.
(2) The prefabricated work piece is loaded into a size-matched mold of the structure shown in fig. 1. As shown in FIG. 2, the axial pressure is set to be 50MPa, and kept constant, and under the action of the axial pressure, the prefabricated ceramic coating area is rapidly heated by pulse current, wherein the current duration, namely the pulse width, is 40ms, the pulse interval is 50ms, the applied voltage is 900V/m, and the local heating speed is 800 ℃/min. And (3) preparing a compact alumina ceramic coating on the surface of the workpiece after the pulse current sintering is finished, wherein the obtained workpiece with the compact alumina ceramic coating on the surface is recorded as a finished workpiece.
Example 2
The preparation method of this example was the same as that of example 1, except that the axial pressure was 45MPa.
Example 3
The preparation method of this example was the same as that of example 1, except that the axial pressure was 55MPa.
Example 4
The preparation of this example was identical to that of example 1, except that the current duration was 35ms and the pulse interval was 100ms.
Example 5
The preparation of this example was identical to that of example 1, except that the current duration was 45ms and the pulse interval was 20ms.
Comparative example 1
The preparation method of this comparative example was the same as that of example 1, except that the axial pressure was 0MPa.
Comparative example 2
The preparation method of this comparative example was the same as that of example 1, except that only axial pressure was applied and pulse current sintering was not started.
Comparative example 3
The preparation method of this comparative example was the same as that of example 1, except that the pre-ceramic coating region was heated at a constant 900V current.
Comparative example 4
The preparation method of this comparative example was the same as that of example 1 except that the powdery raw material of the alumina ceramic coating was charged into a size-matched mold of the structure shown in fig. 1, and the pulse current sintering time was the same as that of example 1.
The average porosities of the ceramic coatings prepared in examples 1 to 5 and comparative examples 1 to 4, that is, five points on the upper, lower, left, right and middle of the ceramic coating were sampled and tested, and then the average was calculated as the average porosities, and the test results are shown in table 1.
TABLE 1 conditions and average porosities of the ceramic coatings prepared in examples 1-5 and comparative examples 1-4
From the preparation of examples 1-5, a dense ceramic coating that is nearly pore free can be prepared when the applied pressure and pulsed current match, such as in examples 1-3. The pulse current flow in example 4 was low, the local heating rate was slow compared to examples 1-3, and the coating densification was low. The pulse current of example 5 was too high and the local temperature rise was too fast and the coating densification was low compared to examples 1-3.
From the preparation of comparative examples 1-2, the compactness of the coating cannot be improved without pulse current or without external pressure, and the average porosity of the coating also increases especially without external pressure.
From the preparation of comparative example 3, the direct application of a constant voltage resulted in severe damage to the coating, cracking, ablation, deformation, and even damage to the workpiece in severe areas, while deformation of the workpiece surface occurred.
From the preparation of comparative example 4, the direct application of raw material particles to the preformed coating layer does not produce a satisfactory coating layer, and due to the effect of the applied pressure, the partial raw material is compacted and sintered to a ceramic state after the pulse current is applied, while the other raw material positions remain in the original state except for adhesion, so that a complete coating layer cannot be formed.
For purposes of this disclosure, the terms "one embodiment," "some embodiments," "example," "a particular example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (10)
1. A method for preparing a dense ceramic coating, comprising the steps of:
(1) Preparing a prefabricated ceramic coating on the surface of a workpiece, and marking the obtained workpiece with the prefabricated ceramic coating on the surface as a prefabricated workpiece;
(2) And loading the prefabricated workpiece into a die, and performing pulse current sintering under the action of axial pressure to obtain a workpiece with the surface provided with the compact ceramic coating, which is recorded as a finished workpiece.
2. The method of claim 1, wherein in step (1), the preformed ceramic coating is prepared by thermal spraying, sol-gel, physical vapor deposition, or chemical vapor deposition.
3. The method for producing a dense ceramic coating according to claim 1, wherein the axial pressure in step (2) is 45-55MPa.
4. The method of claim 1, wherein in step (2), the local heating rate is 500-1000 ℃/min.
5. The method of claim 1, wherein in step (2), the pulse width is 35-45ms and the pulse interval is 20-100ms.
6. The method of claim 5, wherein in step (2), the pulse width is 38-42ms and the pulse interval is 40-60ms.
7. The method for producing a dense ceramic coating according to claim 1 or 5, wherein the pulse current sintering time in step (2) is 1 to 20 minutes.
8. The method for producing a dense ceramic coating according to claim 1, wherein in the step (2), the mold comprises a hot press mold having a cavity for accommodating the prefabricated work and an opening at an upper end and/or a lower end, and an upper pressing mold and a lower supporting mold disposed opposite to each other, the upper pressing mold and/or the lower supporting mold being slidable in the cavity of the hot press mold, the upper pressing mold and/or the lower supporting mold being connected to a driving device, the upper pressing mold and the lower supporting mold being connected to a pulse power source.
9. A dense ceramic coating obtained by the preparation method of any one of claims 1 to 8.
10. A chemical vapor deposition apparatus having the dense ceramic coating of claim 9 disposed on an inner wall of a process chamber of the chemical vapor deposition apparatus.
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