CN110592555B - Preparation method of nano tungsten-based ablation-resistant coating - Google Patents

Preparation method of nano tungsten-based ablation-resistant coating Download PDF

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CN110592555B
CN110592555B CN201911008445.3A CN201911008445A CN110592555B CN 110592555 B CN110592555 B CN 110592555B CN 201911008445 A CN201911008445 A CN 201911008445A CN 110592555 B CN110592555 B CN 110592555B
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nano tungsten
coating
graphite
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李文生
翟海民
成波
何东青
张富邦
胡春莲
张绍兵
安国升
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Lanzhou University of Technology
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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
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    • 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
    • C23C16/22—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 deposition of inorganic material, other than metallic material
    • C23C16/24—Deposition of silicon only
    • 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
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    • C23C24/00—Coating starting from inorganic powder
    • C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
    • C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
    • C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
    • C23C24/087—Coating with metal alloys or metal elements only
    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/32—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer
    • C23C28/322—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one pure metallic layer only coatings of metal elements only
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/30—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer
    • C23C28/34—Coatings combining at least one metallic layer and at least one inorganic non-metallic layer including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates

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Abstract

The invention discloses a preparation method of a nano tungsten-based ablation-resistant coating, which comprises the steps of firstly depositing a graphite-like carbon film on the surface of carbon steel by using a double-carbon-source gaseous chemical codeposition device, then loading the carbon steel into a high-pressure reducing atmosphere treatment furnace for film-based interface strengthening treatment, then flatly paving a single-layer carbon fiber felt on the surface of a graphite-like carbon film carbon steel substrate, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, then repeating the steps until the coating reaches the prefabricated thickness, carrying out compressive stress treatment, and finally carrying out multi-frequency induction surface treatment to finally obtain the nano tungsten-based ablation-resistant coating. The method has the advantages of high control precision of the thickness of the coating, strong process stability and repeatability, and realization of strong interface and high performance of the nano tungsten-based ablation-resistant coating.

Description

Preparation method of nano tungsten-based ablation-resistant coating
Technical Field
The invention relates to the technical field of preparation of ablation-resistant coatings, in particular to a preparation method of a nano tungsten-based ablation-resistant coating.
Background
The high-temperature ablation resistance of the deck structural member used in industries such as ships, armored vehicles, aircrafts and the like is a key index for evaluating the service performance of the deck structural member. The coating technology is an economic and effective means for improving the high-temperature ablation resistance of the deck structural member, but a weak interface is easy to crack and damage under high-temperature thermal stress. Therefore, a new method is found, and the improvement of the interface strength between the layer and the substrate is very important while the high-temperature ablation resistance is enhanced.
Disclosure of Invention
The invention provides a preparation method of a nano tungsten-based ablation-resistant coating, aiming at the current situation of the research and development field that the problem that a weak interface is easy to crack and damage under high-temperature thermal stress by common means is difficult to effectively solve. The method has the advantages of high control precision of the thickness of the coating, strong process stability and repeatability, and realization of strong interface and high performance of the ablation-resistant coating.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a nano tungsten-based ablation-resistant coating comprises the following steps:
1) depositing a graphite-like carbon film on the surface of the carbon steel by using a double carbon source; then carrying out film-based interface strengthening treatment in a reducing atmosphere to obtain a graphite-like carbon film carbon steel matrix;
2) flatly paving a single-layer carbon fiber felt on the surface of a graphite-like carbon film carbon steel substrate, and spraying nano tungsten powder on the surface of the single-layer carbon fiber felt; then, paving a single-layer carbon fiber felt and spraying nano tungsten powder, and repeating the steps until the prefabricated thickness of the coating is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) performing compressive stress treatment on the prefabricated nano tungsten-based coating, and finally performing multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
As a further improvement of the invention, the carbon steel is a No. 45 carbon steel.
As a further improvement of the invention, the surface deposition of the graphite-like carbon film is carried out in a dual-carbon-source gaseous chemical co-deposition device; the carbon source of the double-carbon-source gaseous chemical codeposition device is methane and acetylene, the deposition temperature is 840-1020 ℃, and the thickness of the graphite-like carbon film is 1.1-2.6 microns.
As a further improvement of the present invention, the film-based interface strengthening treatment is carried out in a high-pressure reducing atmosphere treatment furnace; the high-pressure reducing atmosphere treatment furnace is a mixed gas of hydrogen and carbon monoxide with a volume two to one ratio, the air pressure is 2.4-4.5 times of the standard atmospheric pressure, and the treatment temperature is 395-520 ℃.
As a further improvement of the invention, the cross section diameter of the carbon fiber of the single-layer carbon fiber felt is 86 nanometers, the grid size of the fiber felt is 169 nanometers by 172 nanometers, and the average thickness is 105 nanometers.
As a further improvement of the invention, the nano tungsten powder is sprayed by adopting a medium-temperature high-speed pneumatic frequency vibration spraying device; the medium-temperature high-speed pneumatic frequency vibration spraying device is characterized in that a gas medium is helium, the flow rate is 286-363 m/s, the temperature is 465-579 ℃, the vibration frequency of a spray gun is 12-23 Hz, and the single spraying thickness is 160 nanometers.
As a further improvement of the invention, the coating preparation thickness satisfies the following conditions: the number of the carbon fiber felt and the nano tungsten layers is 7-11.
As a further improvement of the invention, the pressure stress treatment temperature is 342-417 ℃, and the pressure is 45-57 MPa.
As a further improvement of the invention, the temperature of the multi-frequency induction surface treatment is 1740-1930 ℃.
As a further improvement of the invention, the surface hardness of the prepared nano tungsten-based ablation-resistant coating is more than or equal to 67HRC, the interface bonding strength is more than or equal to 260MPa, the coating thickness error is less than or equal to 0.34 micrometer, and the propane flame ablation coating speed at 1100 ℃ is less than or equal to 0.01 micrometer/hour.
Compared with the prior art, the invention has the following characteristics and advantages:
firstly, depositing a graphite-like carbon film on the surface of 45# carbon steel by using a dual-carbon-source gaseous chemical codeposition device, then loading the carbon film into a high-pressure reducing atmosphere treatment furnace for strengthening a film-base interface, flatly paving a single-layer carbon fiber felt on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, then repeating the steps until the coating preset thickness is reached, carrying out compressive stress treatment, and finally carrying out multi-frequency induction surface treatment; a graphite-like carbon film is deposited on the surface of a carbon steel substrate, and a nano tungsten-based coating is arranged on the surface of the graphite-like carbon film; the nano tungsten-based coating is formed by spraying single-layer carbon fiber felts and nano tungsten powder at intervals in a laminated mode, wherein the double-carbon-source gaseous chemical codeposition device increases the density and the interface binding force of the graphite-like carbon film through the synergistic effect of two carbon sources. The uniform composition of the single-layer carbon fiber felt and the nano tungsten powder is beneficial to forming a strong tungsten carbide nano crystal boundary and optimizing the fine grain strengthening effect. The multi-frequency induction surface treatment adopts multi-frequency skin current to realize the shrinkage densification and interface strengthening of the ultra-thin and ultra-hard coating. The surface hardness of the prepared nano tungsten-based ablation-resistant coating is greater than or equal to 67HRC, the interface bonding strength is greater than or equal to 260MPa, the coating thickness error is less than or equal to 0.34 micrometer, and the propane flame ablation coating speed at 1100 ℃ is less than or equal to 0.01 micrometer per hour.
Furthermore, the transition film layer strengthening, the carbon nanofiber-tungsten powder composite technology and the multi-frequency induction densification technology are adopted, so that the advantages of good thermal conductivity and high-temperature strength of the carbon fibers and tungsten are fully exerted, and the key means for effectively solving the problem that a weak interface is easy to crack and damage under high-temperature thermal stress is provided.
Furthermore, in the process of preparing the nano tungsten-based ablation-resistant coating, in order to solve the problem that a weak interface is easy to crack and damage under high-temperature thermal stress, the invention adopts a transition film layer strengthening and nano carbon fiber-tungsten powder compounding technology and a multi-frequency induction densification technology.
Detailed Description
The invention relates to a preparation method of a nano tungsten-based ablation-resistant coating, which comprises the following steps:
1) depositing a graphite-like carbon film on the surface of 45# carbon steel by using a dual-carbon-source gaseous chemical codeposition device, wherein the carbon sources are methane and acetylene, the deposition temperature is 840-1020 ℃, the thickness of the graphite-like carbon film is 1.1-2.6 microns, then placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 2.4-4.5 times of the standard atmospheric pressure, and the treatment temperature is 395-520 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 286-363 m/s, the temperature is 465-579 ℃, the vibration frequency of a spray gun is 12-23 Hz, the single spraying thickness is 160 nanometers, and then repeating the steps for 7-11 times until the coating prefabrication thickness is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 342-417 ℃ and 45-57 MPa pressure stress treatment, and finally carrying out 1740-1930 ℃ multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
The method of the present invention is described in detail below with reference to specific examples.
Example 1
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 840 ℃, the thickness of the graphite-like carbon film is 1.1 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 2.4 times of the standard atmospheric pressure, and the treatment temperature is 395 ℃, so that a graphite-like carbon film 45# carbon steel substrate is obtained;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 286 meters per second, the temperature is 465 ℃, the vibration frequency of a spray gun is 12 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 7 times until the prefabricated thickness of the coating is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 342 ℃ and 45MPa pressure stress treatment, and finally carrying out 1740 ℃ multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
Example 2
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 850 ℃, the thickness of the graphite-like carbon film is 1.3 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, wherein the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 2.5 times of the standard atmospheric pressure, and the treatment temperature is 415 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 293 meters per second, the temperature is 479 ℃, the vibration frequency of a spray gun is 13 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 8 times until the coating prefabrication thickness is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 357-47 MPa pressure stress treatment, and finally carrying out 1760-DEG C multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
Example 3
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 860 ℃, the thickness of the graphite-like carbon film is 1.5 microns, then placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 2.6 times of the standard atmospheric pressure, and the treatment temperature is 420 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 298 m/s, the temperature is 489 ℃, the vibration frequency of a spray gun is 16 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 9 times until the coating prefabrication thickness is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing die to perform 367 ℃ and 48MPa pressure stress treatment, and finally performing 1790 ℃ multi-frequency induction surface treatment to finally obtain the nano tungsten-based ablation-resistant coating.
Example 4
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 920 ℃, the thickness of the graphite-like carbon film is 2.1 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, wherein the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 3.5 times of the standard atmospheric pressure, and the treatment temperature is 420 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 313 meters per second, the temperature is 579 ℃, the vibration frequency of a spray gun is 16 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 9 times until the coating prefabrication thickness is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 417 ℃ and 57MPa compressive stress treatment, and finally carrying out 1930 ℃ multi-frequency induction surface treatment to finally obtain the nano tungsten-based ablation-resistant coating.
The performance parameters of the nano tungsten-based ablation-resistant coating prepared in the examples 1-4 are shown in Table 1:
TABLE 1
Figure BDA0002243462970000071
From the above table, the surface hardness of the nano tungsten-based ablation-resistant coating prepared by the method is greater than or equal to 67HRC, the interface bonding strength is greater than or equal to 260MPa, the coating thickness error is less than or equal to 0.34 micrometer, and the propane flame ablation coating speed at 1100 ℃ is less than or equal to 0.01 micrometer/hour.
Example 5
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 1020 ℃, the thickness of the graphite-like carbon film is 2.6 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, wherein the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 2.4 times of the standard atmospheric pressure, and the treatment temperature is 395 ℃, so that a graphite-like carbon film 45# carbon steel substrate is obtained;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 286 meters per second, the temperature is 465 ℃, the vibration frequency of a spray gun is 23 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 11 times until the prefabricated thickness of the coating is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 417 ℃ and 45MPa pressure stress treatment, and finally carrying out 1740 ℃ multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
Example 6
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 920 ℃, the thickness of the graphite-like carbon film is 1.7 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, wherein the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 2.8 times of the standard atmospheric pressure, and the treatment temperature is 510 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel basal body of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 353 meters per second, the temperature is 529 ℃, the vibration frequency of a spray gun is 19 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 10 times until the prefabricated thickness of the coating is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 407 ℃ and 52MPa pressure stress treatment, and finally carrying out 1830 ℃ multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
Example 7
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 1000 ℃, the thickness of the graphite-like carbon film is 2.4 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, wherein the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 3.5 times of the standard atmospheric pressure, and the treatment temperature is 450 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 363 meters per second, the temperature is 579 ℃, the vibration frequency of a spray gun is 23 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 8 times until the coating prefabrication thickness is reached to obtain a prefabricated nano tungsten-based coating;
3) and placing the prefabricated nano tungsten-based coating in a warm-pressing mold for carrying out 397 ℃ and 47MPa pressure stress treatment, and finally carrying out 1840 ℃ multi-frequency induction surface treatment to finally obtain the nano tungsten-based ablation-resistant coating.
Example 8
1) Depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 965 ℃, the thickness of the graphite-like carbon film is 2.5 microns, then, the graphite-like carbon film is loaded into a high-pressure reducing atmosphere treatment furnace to carry out film-base interface strengthening treatment, the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 3.6 times of the standard atmospheric pressure, and the treatment temperature is 486 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 363 meters per second, the temperature is 479 ℃, the vibration frequency of a spray gun is 23 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 11 times until the coating prefabrication thickness is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 417 ℃ and 45MPa pressure stress treatment, and finally carrying out 1740 ℃ multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
Example 9
The invention relates to a preparation method of a nano tungsten-based ablation-resistant coating, which comprises the following steps:
1) depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 840 ℃, the thickness of the graphite-like carbon film is 1.1 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 2.4 times of the standard atmospheric pressure, and the treatment temperature is 395 ℃, so that a graphite-like carbon film 45# carbon steel substrate is obtained;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 286 meters per second, the temperature is 465 ℃, the vibration frequency of a spray gun is 12 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 7 times until the prefabricated thickness of the coating is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 342 ℃ and 45MPa pressure stress treatment, and finally carrying out 1740 ℃ multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
Example 10
The invention relates to a preparation method of a nano tungsten-based ablation-resistant coating, which comprises the following steps:
1) depositing a graphite-like carbon film on the surface of 45# carbon steel by using a double-carbon-source gaseous chemical codeposition device, wherein carbon sources are methane and acetylene, the deposition temperature is 1020 ℃, the thickness of the graphite-like carbon film is 2.6 microns, then, placing the carbon film into a high-pressure reducing atmosphere treatment furnace to perform film-base interface strengthening treatment, wherein the atmosphere is a mixed gas of hydrogen and carbon monoxide with two volume ratios, the air pressure is 4.5 times of the standard atmospheric pressure, and the treatment temperature is 520 ℃, so as to obtain a graphite-like carbon film 45# carbon steel substrate;
2) flatly paving a single-layer carbon fiber felt with the cross section diameter of 86 nanometers, the grid size of 169 nanometers by 172 nanometers and the average thickness of 105 nanometers on the surface of a 45# carbon steel substrate of the graphite-like carbon film, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, wherein a gas medium is helium, the flow rate is 363 meters per second, the temperature is 579 ℃, the vibration frequency of a spray gun is 23 Hz, the single spraying thickness is 160 nanometers, and repeating the steps for 11 times until the coating prefabrication thickness is reached to obtain a prefabricated nano tungsten-based coating;
3) and (3) placing the prefabricated nano tungsten-based coating in a warm-pressing mold, carrying out 417 ℃ and 57MPa compressive stress treatment, and finally carrying out 1930 ℃ multi-frequency induction surface treatment to finally obtain the nano tungsten-based ablation-resistant coating.
The performance parameters of the nano tungsten-based ablation-resistant coating prepared in the examples 5-10 are shown in Table 2:
TABLE 2
Figure BDA0002243462970000111
Figure BDA0002243462970000121
The method comprises the steps of firstly depositing a graphite-like carbon film on the surface of carbon steel by using a dual-carbon-source gaseous chemical codeposition device, then loading the carbon steel into a high-pressure reducing atmosphere treatment furnace for strengthening a film-base interface, then flatly paving a single-layer carbon fiber felt on the surface of a graphite-like carbon film carbon steel substrate, spraying nano tungsten powder on the surface of the single-layer carbon fiber felt by using a medium-temperature high-speed pneumatic frequency vibration spraying device, then repeating the steps until the coating reaches the prefabricated thickness, carrying out compressive stress treatment, and finally carrying out multi-frequency induction surface treatment to finally obtain the nano tungsten-based burning-resistant coating. The method has the advantages of high control precision of the thickness of the coating, strong process stability and repeatability, and realization of strong interface and high performance of the nano tungsten-based ablation-resistant coating.
By researching the relationship among the parameters of dual-carbon source gaseous chemical codeposition, the medium-temperature high-speed pneumatic frequency vibration spraying process, the multi-frequency induction surface treatment technology, the interface of the nano tungsten-based ablation-resistant coating and the high-temperature ablation-resistant performance, the method comprises the following steps: for the nano tungsten-based ablation-resistant coating, optimal dual-carbon-source gaseous chemical codeposition parameters with high interface strength and high-temperature ablation resistance are kept, a medium-temperature high-speed pneumatic frequency vibration spraying process and a multi-frequency induction surface treatment technology are adopted, and the nano tungsten-based ablation-resistant coating is obtained.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and these improvements and modifications should also be construed as the protection scope of the present invention.

Claims (9)

1. A preparation method of a nano tungsten-based ablation-resistant coating is characterized by comprising the following steps:
1) depositing a graphite-like carbon film on the surface of the carbon steel by using a double carbon source; then carrying out film-based interface strengthening treatment in a reducing atmosphere to obtain a graphite-like carbon film carbon steel matrix;
2) flatly paving a single-layer carbon fiber felt on the surface of a graphite-like carbon film carbon steel substrate, and spraying nano tungsten powder on the surface of the single-layer carbon fiber felt; then, paving a single-layer carbon fiber felt and spraying nano tungsten powder, and repeating the steps until the prefabricated thickness of the coating is reached to obtain a prefabricated nano tungsten-based coating;
the nano tungsten powder is sprayed by adopting a medium-temperature high-speed pneumatic frequency vibration spraying device; the medium-temperature high-speed pneumatic frequency vibration spraying device is characterized in that a gas medium of the medium-temperature high-speed pneumatic frequency vibration spraying device is helium, the flow rate is 286-363 m/s, the temperature is 465-579 ℃, the vibration frequency of a spray gun is 12-23 Hz, and the single spraying thickness is 160 nanometers;
3) and (3) performing compressive stress treatment on the prefabricated nano tungsten-based coating, and finally performing multi-frequency induction surface treatment to obtain the nano tungsten-based ablation-resistant coating.
2. The method of claim 1, wherein the carbon steel is 45# carbon steel.
3. The method of claim 1, wherein the surface deposition of the graphite-like carbon film is performed in a dual-carbon source gaseous chemical co-deposition apparatus; the carbon source of the double-carbon-source gaseous chemical codeposition device is methane and acetylene, the deposition temperature is 840-1020 ℃, and the thickness of the graphite-like carbon film is 1.1-2.6 microns.
4. The method of claim 1, wherein the film-based interface strengthening treatment is performed in a high-pressure reducing atmosphere treatment furnace; the high-pressure reducing atmosphere treatment furnace is a mixed gas of hydrogen and carbon monoxide with a volume two to one ratio, the air pressure is 2.4-4.5 times of the standard atmospheric pressure, and the treatment temperature is 395-520 ℃.
5. The method of claim 1, wherein the carbon fiber cross-sectional diameter of the single layer carbon fiber mat is 86 nm, the fiber mat mesh size is 169 nm by 172 nm, and the average thickness is 105 nm.
6. The method of claim 1, wherein the coating is prepared to a thickness of: the number of the carbon fiber felt and the nano tungsten layers is 7-11.
7. The method for preparing the nano tungsten-based ablation-resistant coating according to claim 1, wherein the compressive stress treatment temperature is 342-417 ℃ and the pressure is 45-57 MPa.
8. The method for preparing the nano tungsten-based ablation-resistant coating according to claim 1, wherein the multi-frequency induction surface treatment temperature is 1740-1930 ℃.
9. The method of any one of claims 1 to 8, wherein the surface hardness of the prepared nano tungsten-based ablation-resistant coating is not less than 67HRC, the interface bonding strength is not less than 260MPa, the coating thickness error is not more than 0.34 micron, and the propane flame ablation coating rate at 1100 ℃ is not more than 0.01 micron/hour.
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