CN114774850A - Porous material vapor deposition method and device - Google Patents
Porous material vapor deposition method and device Download PDFInfo
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- CN114774850A CN114774850A CN202210375994.XA CN202210375994A CN114774850A CN 114774850 A CN114774850 A CN 114774850A CN 202210375994 A CN202210375994 A CN 202210375994A CN 114774850 A CN114774850 A CN 114774850A
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- porous
- vapor deposition
- porous material
- preform
- deposition method
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/04—Coating on selected surface areas, e.g. using masks
- C23C14/046—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
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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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/54—Controlling or regulating the coating process
- C23C14/541—Heating or cooling of the substrates
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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
- 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
- C23C16/04—Coating on selected surface areas, e.g. using masks
- C23C16/045—Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates
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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
- 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
- C23C16/46—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 characterised by the method used for heating the substrate
Abstract
The invention belongs to the technical field of new material preparation, and relates to a porous material vapor deposition method and a device; the problem of uneven deposition inside and outside the porous material in the vapor deposition process is solved; the porous material vapor deposition method is that the porous preform is heated from the inside of the porous preform, so that the temperature of the porous preform is gradually reduced from the inside to the outside to form a temperature gradient; carrying out vapor deposition under the temperature gradient to prepare a coating layer by layer from inside to outside of the porous prefabricated body or realize densification; the device comprises a vapor deposition furnace, wherein a reaction thermal field structure is arranged in the furnace, a porous prefabricated material is placed in a working area of the reaction thermal field structure, and a heating element is arranged in the porous prefabricated material; the method is used for preparing high-performance coatings on the surfaces of materials to be treated, and carrying out high-temperature pyrolysis deposition and other process links inside porous prefabricated bodies.
Description
Technical Field
The invention belongs to the technical field of new material preparation, and relates to a porous material vapor deposition method and a porous material vapor deposition device.
Background
Porous preform materials include, but are not limited to, carbon fiber soft/hard felt, silicon carbide fiber soft/hard felt, and the like; the inorganic fiber with beta-silicon carbide structure is prepared with organosilicon compound as material and through spinning, carbonization or vapor deposition. Vapor deposition techniques utilize physical and chemical processes that occur in the vapor phase to form functional or decorative metallic, non-metallic, or compound coatings on the surface of a workpiece. The vapor deposition techniques can be classified into chemical vapor deposition, physical vapor deposition, and plasma vapor deposition according to a film formation mechanism.
In the links of preparing a coating or densifying and the like by a porous material through physical or chemical vapor deposition, the obvious condition of internal and external unevenness exists due to high background temperature; the source gas of the coating or the densified material is decomposed in a large amount in the background, the coating or the densified material is preferentially attached to the outside of the porous material to form a dense layer, so that the coating or the densified material cannot or slightly reaches the inside of the porous material, and the coating or densified preparation process is ineffective.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a method and a device for vapor deposition of a porous material. The problem of uneven deposition inside and outside the porous material in the vapor deposition process is solved.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
A porous material vapor deposition method comprises heating from the inside of a porous preform to gradually lower the temperature of the porous preform from the inside to the outside to form a temperature gradient; and carrying out vapor deposition under the temperature gradient to prepare the coating layer by layer from inside to outside of the porous prefabricated body or realize densification.
Preferably, the working area loaded with the porous preform is evacuated to an extreme vacuum state, then protective gas is introduced, and simultaneously heating is performed from the inside of the porous preform, and when a predetermined process temperature is reached, process gas is introduced into the working area for vapor deposition.
Preferably, after the vapor deposition is finished, the porous preform is cooled, and then the working area is pumped to a limit vacuum state.
Preferably, the working area is a closed space.
The device for the porous material vapor deposition method comprises a vapor deposition furnace, wherein a reaction thermal field structure is arranged in the vapor deposition furnace, a porous prefabricated material is placed in a working area of the reaction thermal field structure, and a heating element is arranged in the porous prefabricated material.
Preferably, the heating element is centrally disposed within the porous preform material.
Preferably, the heat generating element is in direct contact with the porous preform material or is placed within the inner tube in indirect contact with the porous preform material.
Preferably, the reaction thermal field structure comprises an outer tube, an inner tube and a sealing flange; the inner pipe is sleeved in the outer pipe, and the outer pipe is connected with the two ends of the inner pipe through sealing flanges; the outer pipe, the inner pipe and the sealing flange jointly form a working area.
Preferably, the sealing flange is connected with a gas channel.
Preferably, the heating element is a resistive heating element or an inductive heating element.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the temperature gradient of the porous material from inside to outside is established in a manner of heating inside the porous material, so that the aim of gradually coating or densifying the porous material from inside to outside is fulfilled.
The invention realizes uniform coating preparation or densification from inside to outside in the porous material through the internal heating type thermal field, and solves the obvious problem of non-uniformity inside and outside in a CVD or PVD mode.
When the coating or the densification is prepared in the porous material, the process gas from the coating or the densification material reaches the decomposition temperature only at the position close to the position to be deposited, so that the utilization rate of the decomposed process gas is effectively improved, the difficulty in recycling the undecomposed process gas is reduced, and the cost control is facilitated.
The internal heating thermal field is beneficial to preparing high-density composite materials based on porous materials, such as carbon-carbon composite materials, carbon ceramic composite materials and the like, and is beneficial to expanding the application of the composite materials based on the porous materials in novel and higher-requirement occasions.
Drawings
FIG. 1 is a schematic view of a thermal field configuration according to the present invention;
in the figure: 1 is a heating element, 2 is an inner tube, 3 is a porous preform material, 4 is an outer tube, and 5 is a sealing flange.
Detailed Description
In order to make the technical problems, technical solutions and beneficial effects to be solved by the present invention clearer, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. 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 technical solution of the present invention is described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
As shown in fig. 1, this embodiment discloses an apparatus for a vapor deposition method of a porous material, which is suitable for a process of preparing a coating or densifying the porous material. The thermal field involved is mainly composed of: the heating element 1, the inner tube 2, the porous preform material 3, the outer tube 4 and the sealing flange 5 are also not explicitly shown in the schematic view since they are not essential to the invention, e.g. temperature measurement, furnace chamber pressure measurement, process/shielding gas channels, mechanical support, etc., and do not represent that these non-essential components are not required in the practice of the invention.
Wherein: the heating element 1 used for generating heat inside the workpiece to be processed includes, but is not limited to, resistive heating (such as silicon carbide rod, silicon molybdenum rod, resistance wire, graphite heating, etc., but not limited to the resistive heating), induction heating (central induction component such as graphite, metal, etc.), and other heating methods. The inner tube 2 can be made of corrosion-resistant materials such as quartz; the porous preform material 3 to be treated includes, but is not limited to, carbon fiber soft/hard felt, silicon carbide fiber soft/hard felt, and the like; the outer tube 4 can be made of various materials such as quartz, stainless steel, etc.
The structure of the thermal field described in this embodiment is shown in fig. 1, in which:
1) the heating element 1 is disposed in the central portion of the porous preform material 3, and the heating element 1 and the porous preform material 3 are isolated by the inner tube 2.
2) The inner wall of the inner tube 2 can be sealed or unsealed, and filled or not filled with protective gas according to the use requirements of different heating elements 1.
3) The outer wall of the inner pipe 2, the inner wall of the outer pipe 4 and the sealing flange 5 form a core working area of the thermal field, the outer wall of the inner pipe 2, the sealing flange 5 and the inner wall of the outer pipe 4 and the sealing flange 5 are sealed through sealing rings, and a process/protective gas channel, a thermocouple channel and a furnace chamber pressure measuring channel are established through being located at a specific position of the sealing flange 5, so that the control of the temperature, the pressure, the gas flow and the like of the core working area of the thermal field is realized.
4) Porous prefabricated body material 3 adheres to in the outer wall of inner tube 2, is located the inner tube 2 outer wall and forms the core workspace of this thermal field with outer tube 4 inner wall, sealing flange 5, and through the design of structure, the gas passage who establishes from sealing flange 5 can be preferentially through porous prefabricated body material 3, promotes process gas's effective utilization.
5) The outer wall of the outer pipe 4 is provided with a heat preservation layer, so that secondary disasters caused by overhigh temperature outside the thermal field due to thermal radiation are avoided.
The thermal field structure controls the pressure in the cavity through the air inlet and outlet; the temperature range of the thermal field structure is 100-1200 ℃; in the embodiment, the internal heating element of the workpiece is connected with the workpiece through the inner pipe, and heat transfer is realized in a radiation and contact heat conduction mode; the internal workpiece heating element may be in direct contact with the workpiece.
The working principle is as follows:
after the porous prefabricated material 3 is loaded in place, a core working area formed by the outer wall of the inner pipe 2, the inner wall of the outer pipe 4 and the sealing flange 5 is vacuumized to the limit through a vacuum system, then protective gas is filled through a gas channel reserved on the sealing flange 5, meanwhile, the heating element 1 heats the system, when the preset process temperature is reached, process gas enters the core working area through the gas channel reserved on the sealing flange 5 according to the set flow and pressure, the coating preparation or densification is realized after decomposition through the porous prefabricated material 3, and decomposition byproducts and undecomposed process gas are discharged from the core working area through the sealing flange 5. This process is continued until the porous preform material 3 meets the set process requirements. And then, the process air inlet is closed, and the heating system is cooled according to the process requirement. After the set temperature is reached, the evacuation system initiates evacuation of the core work area to a limit vacuum.
The process gas includes but is not limited to carbon source simple substance or mixed gas such as methane, acetylene and the like; the protective gas includes but is not limited to inert simple substance or mixed gas such as argon, nitrogen and the like; the temperature of the porous prefabricated body is gradually reduced from inside to outside, and the temperature gradient can be adjusted according to the material to be deposited or pyrolyzed; the internal heating mode of the workpiece is realized, and the temperature gradually decreases along with the distance from the body center of the workpiece; the porous prefabricated body is used for preparing a coating layer from inside to outside layer by layer or realizing densification.
The thermal field structure realizes the technical processes of coating preparation, pyrolysis, deposition and the like of the material to be treated in a mode of heating in the material to be treated, and is used for preparing a high-performance coating on the surface of the material to be treated and carrying out high-temperature pyrolysis deposition and other technical links in a porous prefabricated body.
The device is suitable for thermal equipment for preparing coatings and depositing pyrolysis substances on the surfaces of porous preforms under the conditions of vertical/horizontal type, high temperature, positive pressure/negative pressure and process gas/protective gas.
The above is a further detailed description of the present invention with reference to specific preferred embodiments, which should not be considered as limiting the invention to the specific embodiments described herein, but rather as a matter of simple derivation or substitution within the scope of the invention as defined by the appended claims, it will be understood by those skilled in the art to which the invention pertains.
Claims (10)
1. A porous material vapor deposition method is characterized in that a porous preform is heated from the inside of the porous preform, so that the temperature of the porous preform is gradually reduced from the inside to the outside to form a temperature gradient; and carrying out vapor deposition under the temperature gradient to prepare the coating layer by layer from inside to outside of the porous prefabricated body or realize densification.
2. A porous material vapor deposition method according to claim 1, wherein the working region loaded with the porous preform is evacuated to an extreme vacuum state, and then a protective gas is introduced, and simultaneously heated from the inside of the porous preform, and when a predetermined process temperature is reached, a process gas is introduced into the working region to perform vapor deposition.
3. The vapor deposition method of a porous material according to claim 2, wherein after the vapor deposition is finished, the porous preform is cooled, and then the working area is pumped to a limit vacuum state.
4. A porous material vapor deposition process according to claim 2, wherein said working zone is a closed space.
5. An apparatus for use in a method of vapour deposition of a porous material according to any of claims 1 to 4, comprising a vapour deposition furnace in which is disposed a reactive thermal field structure having a porous precursor material disposed in a working region thereof, wherein the porous precursor material has heating elements disposed therein.
6. An apparatus for a vapor deposition method of a porous material according to claim 5, wherein the heat generating element is disposed at the center inside the porous preform material.
7. An apparatus for a vapor deposition method of porous material according to claim 5, wherein the heat generating element is in direct contact with the porous preform material or is placed inside the inner tube in indirect contact with the porous preform material.
8. The apparatus according to claim 5, wherein the reaction thermal field structure comprises an outer tube, an inner tube and a sealing flange; the inner pipe is sleeved in the outer pipe, and the outer pipe is connected with the two ends of the inner pipe through sealing flanges; the outer pipe, the inner pipe and the sealing flange jointly form a working area.
9. An apparatus for a vapor deposition method of porous material according to claim 8, wherein the sealing flange is connected with a gas passage.
10. The apparatus according to claim 5, wherein the heating element is a resistive heating element or an inductive heating element.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210375994.XA CN114774850A (en) | 2022-04-11 | 2022-04-11 | Porous material vapor deposition method and device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210375994.XA CN114774850A (en) | 2022-04-11 | 2022-04-11 | Porous material vapor deposition method and device |
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| Publication Number | Publication Date |
|---|---|
| CN114774850A true CN114774850A (en) | 2022-07-22 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202210375994.XA Pending CN114774850A (en) | 2022-04-11 | 2022-04-11 | Porous material vapor deposition method and device |
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| CN (1) | CN114774850A (en) |
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2022
- 2022-04-11 CN CN202210375994.XA patent/CN114774850A/en active Pending
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Address after: No. 8 Beige Street, Xiaohe Industrial Park, Shanxi Transformation Comprehensive Reform Demonstration Zone, Taiyuan City, Shanxi Province, 030032 Applicant after: CETC SHANXI BRANCH OF NEW ENERGY Co. Address before: 030032 No. 5, Tanghuai Road, Tanghuai Park, comprehensive reform demonstration area, Xiaodian District, Taiyuan City, Shanxi Province Applicant before: CETC SHANXI BRANCH OF NEW ENERGY Co. |
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