CN112430802A - Method and device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings - Google Patents
Method and device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings Download PDFInfo
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- CN112430802A CN112430802A CN202011071362.1A CN202011071362A CN112430802A CN 112430802 A CN112430802 A CN 112430802A CN 202011071362 A CN202011071362 A CN 202011071362A CN 112430802 A CN112430802 A CN 112430802A
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- 238000004140 cleaning Methods 0.000 title claims abstract description 125
- 238000000576 coating method Methods 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 101
- 229910000951 Aluminide Inorganic materials 0.000 title claims abstract description 97
- -1 fluorine ions Chemical class 0.000 title claims abstract description 73
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 49
- 239000011737 fluorine Substances 0.000 title claims abstract description 49
- 239000011248 coating agent Substances 0.000 claims abstract description 102
- 239000007789 gas Substances 0.000 claims description 203
- 238000006243 chemical reaction Methods 0.000 claims description 157
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 124
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 98
- 239000001257 hydrogen Substances 0.000 claims description 93
- 229910052739 hydrogen Inorganic materials 0.000 claims description 93
- 229910052786 argon Inorganic materials 0.000 claims description 62
- 238000005269 aluminizing Methods 0.000 claims description 48
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 43
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 41
- 238000010438 heat treatment Methods 0.000 claims description 40
- 238000004321 preservation Methods 0.000 claims description 40
- 229910002804 graphite Inorganic materials 0.000 claims description 36
- 239000010439 graphite Substances 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 35
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 35
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 35
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 34
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 20
- 229910052782 aluminium Inorganic materials 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 16
- 150000002431 hydrogen Chemical class 0.000 claims description 16
- 238000011049 filling Methods 0.000 claims description 15
- 239000012670 alkaline solution Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 11
- 239000002184 metal Substances 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 3
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 37
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 12
- 239000011253 protective coating Substances 0.000 abstract description 12
- 229910045601 alloy Inorganic materials 0.000 abstract description 9
- 239000000956 alloy Substances 0.000 abstract description 9
- 229910052759 nickel Inorganic materials 0.000 abstract description 6
- 239000013078 crystal Substances 0.000 abstract description 5
- 230000003749 cleanliness Effects 0.000 abstract description 4
- 238000012545 processing Methods 0.000 abstract description 4
- 229910000601 superalloy Inorganic materials 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 13
- 239000012071 phase Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- IZMHKHHRLNWLMK-UHFFFAOYSA-M chloridoaluminium Chemical compound Cl[Al] IZMHKHHRLNWLMK-UHFFFAOYSA-M 0.000 description 3
- HRLHOWWCFUKTIY-UHFFFAOYSA-L dichloroalumanylium Chemical compound Cl[Al+]Cl HRLHOWWCFUKTIY-UHFFFAOYSA-L 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000943 NiAl Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910010342 TiF4 Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- UOUJSJZBMCDAEU-UHFFFAOYSA-N chromium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Cr+3].[Cr+3] UOUJSJZBMCDAEU-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000011268 retreatment Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000012720 thermal barrier coating Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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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
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0227—Pretreatment of the material to be coated by cleaning or etching
- C23C16/0245—Pretreatment of the material to be coated by cleaning or etching by etching with a plasma
-
- 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
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
- C23C10/08—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases only one element being diffused
-
- 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
- C23C16/22—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
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
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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
- C23C16/54—Apparatus specially adapted for continuous coating
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Inorganic Chemistry (AREA)
- Turbine Rotor Nozzle Sealing (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
The invention discloses a method and a device for cleaning fluorine ions of a blade with a complex inner cavity and preparing an aluminide coating. The two processes are integrally completed in the CVD equipment, the CVD equipment does not need to be opened, the blade does not need to be taken out, the processing time can be saved, the secondary pollution to the blade caused by taking out the blade midway can be avoided, the method is flexible and controllable, the prepared aluminide coating has high cleanliness, and the blade cannot be damaged. The method is particularly suitable for preparing the nickel-based single crystal superalloy guider blade with a complex inner cavity structure, the inner cavity of a high-pressure turbine blade and the high-temperature protective coating on the surface by a chemical vapor deposition method, and is also suitable for preparing the protective coatings of other high-temperature alloy parts.
Description
Technical Field
The invention relates to the technical field of high-temperature alloy coatings and preparation thereof, in particular to a method and a device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings.
Background
The nickel-based high-temperature single crystal alloy has excellent high-temperature mechanical property and is the main material for manufacturing the blades of advanced aircraft engines and gas turbines at present. Because of the extremely harsh working environment of the engine, the alloy is required to have good high-temperature mechanical properties, and excellent high-temperature oxidation resistance and thermal corrosion resistance. However, in practical applications, it is difficult for the same alloy to satisfy multiple properties simultaneously. To resolve this conflict, the most effective method is to use high temperature protective coating technology.
In the production process of the blade, when the ceramic mould shell is removed and the ceramic core is removed from the inner cavity, oxide film layers are respectively generated on the outer surface and the inner cavity surface of the blade, and the existence of the oxide film layers can hinder the internal diffusion of aluminum element in the chemical vapor deposition aluminizing process and inhibit the formation of an aluminide coating. The outer surface of the blade is cleaned by sand blasting, so that a clean metal surface can be obtained, and the requirements of chemical vapor deposition aluminizing pretreatment are met. Patent publication No. CN104923520A proposes an abrasive flow technique, which utilizes the latest machining process of abrasive medium flowing under pressure to perform deburring, fillet grinding, etc. on the surface of a workpiece to be machined, so as to reduce surface waviness and roughness and achieve the purpose of precision machining. For the blade with a simple inner cavity structure, the inner cavity of the blade can be cleaned by an abrasive particle flow technology. However, for a blade with a complex inner cavity structure (such as a double-wall structure), the inner cavity cannot be cleaned completely due to the narrow passage and small pores of the turbine blade, which may cause the viscous abrasive to be easily remained therein, so that a gas-phase permeation layer is difficult to form in the inner cavity, which brings difficulty in cleaning.
Currently, commonly used aluminizing methods mainly include: pack aluminizing, Vapor Phase Aluminizing (VPA), and chemical vapor deposition aluminizing (CVD). The disadvantage of pack aluminizing is that pack powder is easy to sinter at high temperature, blocking the cooling hole, and it is difficult to accurately guide into the tiny channel of the blade during aluminizing, and it is difficult to prepare ideal protective coating in the inner cavity. The disadvantage of gas phase aluminizing is that although separation of powder from the infiltrated piece is achieved, there are limitations in parameter control. The CVD aluminizing can aluminize an inner cavity with a complex structure in the blade, does not need powder, and can control the growth rate, the structure and the performance of the coating by simultaneously controlling the gas flow under certain temperature and pressure. Therefore, CVD aluminizing is the cleanest of the three processes, and is currently the most widely used process.
The patent with publication number CN105695929A discloses a preparation method of a blade protective coating suitable for a high-Mo-content complex inner cavity structure, which adopts a muffle furnace to carry out blade inner cavity fluorine ion cleaning and gas phase aluminized silicon coating preparation, and the method has the defects that the blade needs to be taken out from the muffle furnace for retreatment in midway, a solid penetrating agent is added, the cleaning and coating preparation can not be integrally treated, the muffle furnace needs to be heated and cooled for multiple times, and the time of the whole treatment process is increased.
Disclosure of Invention
In view of the above, the invention provides a method and a device for cleaning fluorine ions and preparing an aluminide coating of a complex inner cavity blade, which are used for integrally completing cleaning treatment of an oxide film layer of the complex inner cavity blade and preparation of an aluminide protective coating.
The invention provides a method for cleaning fluorine ions of a blade with a complex inner cavity and preparing an aluminide coating, which comprises the following steps:
s1: placing the deoiled and cleaned or sand-blast cleaned blade in a reaction chamber of CVD equipment, and placing an aluminum block with preset quality in a graphite labyrinth in the reaction chamber;
s2: pumping the reaction chamber to a vacuum state, and then filling argon into the reaction chamber to atmospheric pressure to finish the primary cleaning of the blade; repeatedly cleaning for several times;
s3: stopping introducing argon, continuously introducing hydrogen into the reaction chamber, keeping the pressure at a preset pressure, heating the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and keeping the temperature for a first preset time;
s4: after the heat preservation is finished, continuously introducing hydrogen and hydrogen fluoride gas into the reaction chamber, or continuously introducing hydrogen and Freon gas into the reaction chamber, keeping the air pressure at a preset pressure, and continuously preserving the heat for a second preset time; hydrogen and hydrogen fluoride gas or hydrogen and Freon gas enter the cavity inside the blade through the air inlet of the blade tenon, flow out of the air film cooling hole, flow out of the air outlet of the reaction chamber, pass through the alkaline solution pool and then are discharged into the atmosphere;
s5: after the heat preservation is finished, stopping introducing hydrogen fluoride gas or Freon gas, and finishing the cleaning of the fluorine ions in the inner cavity of the blade;
s6: continuously filling hydrogen into the reaction chamber, and discharging residual hydrogen fluoride gas or Freon gas out of the reaction chamber;
s7: under the condition of continuously charging hydrogen, keeping the pressure at a preset pressure, heating the reaction chamber from the first preset temperature to a second preset temperature at a preset heating rate, and keeping the temperature for a first preset time;
s8: after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen and argon gas which pass through the preheating pipeline into the reaction chamber, keeping the pressure at a preset pressure, and continuously preserving the heat for a third preset time; wherein the temperature of the preheating pipeline is a third preset temperature; hydrogen chloride gas, hydrogen gas and argon gas enter the cavity inside the blade through the gas inlet of the blade tenon, flow out of the gas film cooling hole, flow out of the gas outlet of the reaction chamber, pass through the alkaline solution pool and then are discharged into the atmosphere;
s9: and after the heat preservation is finished, stopping introducing hydrogen chloride gas and hydrogen, continuously introducing argon, stopping vacuumizing after the blades are cooled to room temperature along with the reaction chamber, stopping introducing argon after the pressure of the reaction chamber is increased to the atmospheric pressure, opening the chamber, taking the blades, and finishing the preparation of the aluminide coating.
In a possible implementation manner, in the method for cleaning fluorine ions and preparing an aluminide coating on a complex inner cavity blade provided by the invention, in step S3, the introduction of argon is stopped, hydrogen is continuously introduced into the reaction chamber, the pressure is kept at a preset pressure, the reaction chamber is heated from room temperature to a first preset temperature at a preset heating rate, and the temperature is kept for a first preset time, which specifically includes the following steps:
s30: stopping introducing the argon, continuously introducing the hydrogen into the reaction chamber, keeping the air pressure at 15-30 kPa, heating the reaction chamber from room temperature to 950-1000 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
In a possible implementation manner, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, in step S4, after the heat preservation is finished, continuously introducing hydrogen and hydrogen fluoride gas into the reaction chamber, or continuously introducing hydrogen and freon gas into the reaction chamber, so that the air pressure is kept at a preset pressure, and continuously preserving the heat for a second preset time, specifically, the method includes the following steps:
s40: after the heat preservation is finished, continuously introducing hydrogen and hydrogen fluoride gas into the reaction chamber, or continuously introducing hydrogen and Freon gas into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1 h.
In a possible implementation manner, in the method for cleaning fluorine ions and preparing an aluminide coating on a blade with a complex inner cavity, provided by the invention, in step S7, in a state where hydrogen gas is continuously filled, the gas pressure is kept at a preset pressure, the reaction chamber is heated from the first preset temperature to the second preset temperature at a preset heating rate, and the temperature is kept for a first preset time, which specifically includes the following steps:
s70: and under the condition of continuously filling hydrogen, keeping the air pressure at 15-30 kPa, heating the reaction chamber from the first preset temperature to 1000-1100 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
In a possible implementation manner, in the method for cleaning the complex inner cavity blade by using the fluoride ions and preparing the aluminide coating, step S8, after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen gas and argon gas which pass through the preheating pipeline into the reaction chamber, keeping the air pressure at a preset pressure, and continuously preserving the heat for a third preset time; wherein, the temperature of preheating the pipeline is the third preset temperature, specifically includes the following steps:
s80: after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen and argon gas which pass through a preheating pipeline into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1-3 h; wherein the temperature of the preheating pipeline is 200-300 ℃.
In a possible implementation manner, in the method for cleaning the complex inner cavity blade by the fluoride ions and preparing the aluminide coating, the purity of hydrogen, argon and hydrogen chloride gas is 99.9%, and the purity of hydrogen fluoride gas or freon gas is 99.9%.
In a possible implementation manner, in the method for cleaning the fluorine ions of the blade with the complex inner cavity and preparing the aluminide coating, provided by the invention, the flow rate of hydrogen fluoride gas is 0.5L/min to 1L/min, and the ratio of the flow rate of hydrogen fluoride to the flow rate of hydrogen fluoride gas is 10: 1; or,
the flow rate of the Freon gas is 0.5L/min-1L/min, the ratio of the hydrogen flow rate to the flow rate of the Freon gas is 10: 1.
in a possible implementation mode, in the method for cleaning the fluorine ions of the blades with the complex inner cavities and preparing the aluminide coating, provided by the invention, the flow rate of hydrogen chloride gas is 0.5L/min-1L/min;
the ratio of argon flow, hydrogen flow and hydrogen chloride gas flow is 10: 10: 1.
in a possible implementation mode, in the method for cleaning the complex inner cavity blade by using the fluoride ions and preparing the aluminide coating, the thickness of the aluminide coating is 20-50 μm.
The invention also provides a device for cleaning the fluorine ions of the blades with complex inner cavities and preparing the aluminide coating, which comprises the following components: the device comprises a reaction chamber, a graphite labyrinth, a blade tool, an aluminizing channel, a fluorine ion cleaning channel, a gas generation chamber, a thermocouple and a metal mesh; wherein,
the graphite labyrinth and the blade tool are positioned in the reaction chamber, the blade tool is used for installing a blade, the blade is installed above the blade tool, and the blade tool is positioned above the graphite labyrinth; the graphite labyrinth is provided with a labyrinth channel, the labyrinth channel is used for placing an aluminum block, the air outlet of the labyrinth channel is aligned to a tenon of a blade arranged on the blade tool, the air inlet of the labyrinth channel is communicated with an aluminizing channel positioned outside the reaction chamber, the gas generation chamber is positioned on the aluminizing channel, the gas generation chamber is used for placing the aluminum block, the aluminizing channel is used for introducing hydrogen chloride gas, hydrogen gas and argon gas, and the gas in the aluminizing channel passes through the gas generation chamber, then passes through the labyrinth channel and enters the blade from the air outlet of the labyrinth channel;
the fluorine ion cleaning channel is embedded into the aluminized channel at a position between the gas generating chamber and the inlet of the labyrinth channel and penetrates from the center of the graphite labyrinth to the outlet of the labyrinth channel; the fluorine ion cleaning channel is used for introducing hydrogen fluoride gas, hydrogen and argon, or introducing Freon gas, hydrogen and argon;
the metal net is positioned at the air outlet of the fluoride ion cleaning channel and used for preventing carbon generated by the reaction of Freon gas and hydrogen from entering the blade at high temperature;
the thermocouple is positioned on the inner wall of the reaction chamber and is used for measuring the temperature in the reaction chamber;
and an exhaust port for exhausting reaction tail gas is arranged at the bottom of the reaction chamber.
According to the method and the device for cleaning the fluorine ions of the blade with the complex inner cavity and preparing the aluminide coating, the fluorine ions of the inner cavity of the blade are cleaned and the aluminide coating is prepared by a Chemical Vapor Deposition (CVD) method, and the fluorine ions of the inner cavity of the blade are cleaned to remove the residual oxide layer on the wall of the inner cavity, so that conditions are provided for preparing the aluminized coating by a subsequent chemical vapor deposition method. The two processes of fluoride ion cleaning and aluminide coating preparation are all completed by adopting CVD equipment, the CVD equipment does not need to be opened between the two processes, the blade does not need to be taken out, the two processes are integrally completed in the CVD equipment, the treatment time can be saved, the secondary pollution to the blade caused by taking out the blade midway can be avoided, the method is flexible and controllable, the prepared aluminide coating has high cleanliness, and the blade cannot be damaged. The method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating is particularly suitable for preparing the nickel-based single crystal superalloy guider blade with the complex inner cavity structure, the high-pressure turbine blade inner cavity and the surface high-temperature protective coating by a chemical vapor deposition method, and is also suitable for preparing the protective coatings of other high-temperature alloy parts.
Drawings
FIG. 1 is a flow chart of a method for cleaning fluorine ions and preparing an aluminide coating on a complex inner cavity blade provided by the invention;
FIG. 2 is a cross-sectional view of a blade having a complex internal cavity structure;
FIG. 3 is a schematic structural diagram of an apparatus for cleaning fluorine ions and preparing an aluminide coating on a complex inner cavity blade according to the present invention;
FIG. 4 is a second schematic structural diagram of an apparatus for cleaning fluorine ions and preparing an aluminide coating on a blade with a complicated inner cavity according to the present invention.
Description of the drawings: the device comprises an inner wall 1, an impact cooling hole 2, an outer wall 3, a gas film cooling hole 4, an interlayer 5, a blade inner part 6, a reaction chamber 7, a graphite labyrinth 8, a blade tool 9, an aluminizing channel 10, a fluorine ion cleaning channel 11, a gas generation chamber 12, a thermocouple 13, a metal mesh 14, a blade 15, a tenon 16 and an exhaust port 17.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only illustrative and are not intended to limit the present invention.
The invention provides a method for cleaning fluorine ions of a blade with a complex inner cavity and preparing an aluminide coating, which comprises the following steps of:
s1: placing the deoiled and cleaned or sand-blast cleaned blade in a reaction chamber of CVD equipment, and placing an aluminum block with preset quality in a graphite labyrinth in the reaction chamber;
s2: pumping the reaction chamber to a vacuum state, and then filling argon into the reaction chamber to atmospheric pressure to finish the primary cleaning of the blade; repeatedly cleaning for several times;
s3: stopping introducing argon, continuously introducing hydrogen into the reaction chamber, keeping the pressure at a preset pressure, heating the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and keeping the temperature for a first preset time;
s4: after the heat preservation is finished, continuously introducing hydrogen and hydrogen fluoride gas into the reaction chamber, or continuously introducing hydrogen and Freon gas into the reaction chamber, keeping the air pressure at a preset pressure, and continuously preserving the heat for a second preset time; hydrogen and hydrogen fluoride gas or hydrogen and Freon gas enter the cavity inside the blade through the air inlet of the blade tenon, flow out of the air film cooling hole, flow out of the air outlet of the reaction chamber, pass through the alkaline solution pool and then are discharged into the atmosphere;
s5: after the heat preservation is finished, stopping introducing hydrogen fluoride gas or Freon gas, and finishing the cleaning of the fluorine ions in the inner cavity of the blade;
s6: continuously filling hydrogen into the reaction chamber, and discharging residual hydrogen fluoride gas or Freon gas out of the reaction chamber;
s7: under the condition of continuously charging hydrogen, keeping the pressure at a preset pressure, heating the reaction chamber from a first preset temperature to a second preset temperature at a preset heating rate, and keeping the temperature for a first preset time;
s8: after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen and argon gas which pass through the preheating pipeline into the reaction chamber, keeping the pressure at a preset pressure, and continuously preserving the heat for a third preset time; wherein the temperature of the preheating pipeline is a third preset temperature; hydrogen chloride gas, hydrogen gas and argon gas enter the cavity inside the blade through the gas inlet of the blade tenon, flow out of the gas film cooling hole, flow out of the gas outlet of the reaction chamber, pass through the alkaline solution pool and then are discharged into the atmosphere;
s9: and after the heat preservation is finished, stopping introducing hydrogen chloride gas and hydrogen, continuously introducing argon, stopping vacuumizing after the blades are cooled to room temperature along with the reaction chamber, stopping introducing argon after the pressure of the reaction chamber is increased to the atmospheric pressure, opening the chamber, taking the blades, and finishing the preparation of the aluminide coating.
In specific implementation, in the method for cleaning the complex inner cavity blade with the fluorine ions and preparing the aluminide coating, steps S1 to S5 are the process of cleaning the inner cavity of the blade with the fluorine ions by a Chemical Vapor Deposition (CVD) method, and the purpose of cleaning the inner cavity of the blade with the fluorine ions is to remove the residual oxide layer on the wall of the inner cavity and provide conditions for preparing the aluminized coating by a subsequent CVD method. Steps S6 to S9 are processes of preparing an aluminide coating of the inner cavity of the blade by chemical vapor deposition aluminizing. The two processes are all completed by adopting the CVD equipment, the CVD equipment does not need to be opened between the two processes, the blade does not need to be taken out, the two processes are integrally completed in the CVD equipment, the processing time can be saved, the secondary pollution to the blade caused by taking out the blade midway can be avoided, the method is flexible and controllable, the prepared aluminide coating has high cleanliness, and the blade cannot be damaged. The method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating is particularly suitable for preparing the nickel-based single crystal superalloy guider blade with the complex inner cavity structure, the high-pressure turbine blade inner cavity and the surface high-temperature protective coating by a chemical vapor deposition method, and is also suitable for preparing the protective coatings of other high-temperature alloy parts.
Fig. 2 is a sectional view of a blade having a complicated inner cavity structure. Different from a common hollow blade, the complex inner cavity blade is a double-layer wall, a plurality of impingement cooling holes 2 are formed in the inner wall 1 through casting processing, a plurality of air film cooling holes 4 are formed in the outer wall 3 through electric spark processing, and the thickness of the interlayer 5 is about 1 mm. Due to the complex structure of the blade, oxides on the surface of the inner cavity cannot be removed by processing methods such as abrasive flow and the like, and an abrasive medium is difficult to clean, which brings difficulty to the preparation of a subsequent chemical vapor deposition infiltration layer of the inner cavity. The invention cleans the surface of the inner cavity of the blade by adopting fluoride ion cleaning to remove the oxide film layer, thereby providing conditions for preparing the aluminide coating by the subsequent chemical vapor deposition method. The cleaning of the fluorine ions in the inner cavity of the blade is realized through a specific tool design (particularly, refer to the following device part), so that the cleaning atmosphere of the fluorine ions enters the blade interior 6 through cover plates at two ends of the guide vane or the tenon of the turbine blade, and is discharged from the air film cooling hole 4 after passing through the impingement cooling hole 2 and the middle interlayer 5 in sequence. Under the condition of high temperature of 950-1000 ℃, the fluorine ion cleaning atmosphere reacts with the oxide layer to form a gas phase product, so that the fluorine ion cleaning of the inner cavity (the inner part 6 of the blade and the interlayer 5) of the blade is realized. Specifically, the introduced hydrogen fluoride gas can fully react with oxides (mainly aluminum, titanium, chromium oxides and composite oxides thereof) attached to the inner cavity of the blade, and the reaction formula is as follows:
6HF+Al2O3→2AlF3+3H2O
4HF+TiO2→TiF4+2H2O
6HF+Cr2O3→2CrF3+F2+3H2O。
in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, in the preparation process of the aluminide coating, when the substrate (namely the inner cavity surface and the outer surface of the blade) is made of nickel-based high-temperature alloy, the outermost layer/surface layer of the aluminide coating is made of beta-NiAl phase, and a mutual diffusion region is formed between the surface layer and the substrate. Under the high-temperature environment, the NiAl phase can be oxidized, so that a layer of compact alumina is formed on the surface of the surface phase of the aluminide coating, and the high-temperature oxidation resistance of the blade can be improved. After the aluminide coating is prepared by aluminizing by using a chemical vapor deposition method, the MCrAlY coating and the ceramic-based thermal barrier coating can be further prepared on the surface of the aluminide coating.
The following two specific examples are provided to describe the specific parameters and specific conditions of the method for cleaning the complex inner cavity blade by the fluoride ions and preparing the aluminide coating in the specific examples.
Example 1:
in the step S4 of the method for cleaning fluorine ions and preparing an aluminide coating on a complex inner cavity blade according to the present invention, the gas for cleaning fluorine ions continuously introduced into the reaction chamber is hydrogen fluoride gas and hydrogen gas.
In practical implementation, when step S1 in the method for cleaning fluorine ions and preparing an aluminide coating on a complicated inner-cavity blade provided by the invention is executed, 50g to 100g of aluminum blocks can be put into the graphite labyrinth in the reaction chamber. Specifically, the amount of the aluminum block to be put may be determined according to the length of the labyrinth passage of the graphite labyrinth.
In specific implementation, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, in step S3, the introduction of argon is stopped, hydrogen is continuously introduced into the reaction chamber, the pressure is kept at a preset pressure, the reaction chamber is heated from room temperature to a first preset temperature at a preset heating rate, and the temperature is kept for a first preset time, which specifically includes the following steps:
s30: stopping introducing the argon, continuously introducing the hydrogen into the reaction chamber, keeping the air pressure at 15-30 kPa, heating the reaction chamber from room temperature to 950-1000 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
In specific implementation, in the method for cleaning the fluorine ions of the blade with the complex inner cavity and preparing the aluminide coating, provided by the invention, in step S4, after the heat preservation is finished, hydrogen and hydrogen fluoride gas are continuously introduced into the reaction chamber, the air pressure is kept at a preset pressure, and the heat preservation is continuously carried out for a second preset time, which specifically includes the following steps:
s40: after the heat preservation is finished, continuously introducing hydrogen and hydrogen fluoride gas into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1 h.
In the method for cleaning the complex inner cavity blade with fluoride ions and preparing the aluminide coating, in step S4, the flow rate of the hydrogen fluoride gas introduced into the reaction chamber may be controlled within a range of 0.5L/min to 1L/min, and the ratio of the hydrogen flow rate to the hydrogen fluoride gas flow rate may be 10: 1, whereby the flow rate of hydrogen to the reaction chamber can also be determined.
In the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, in the step S6, hydrogen is continuously filled into the reaction chamber, so that the residual hydrogen fluoride gas is discharged out of the reaction chamber, and the influence of the residual hydrogen fluoride gas on the subsequent preparation of the aluminide coating can be avoided.
In a specific implementation, in the method for cleaning fluorine ions and preparing an aluminide coating on a blade with a complex inner cavity provided by the invention, in step S7, in a state of continuously filling hydrogen, the pressure is kept at a preset pressure, the reaction chamber is heated from the first preset temperature to the second preset temperature at a preset heating rate, and the temperature is kept for a first preset time, which specifically includes the following steps:
s70: keeping the air pressure at 15-30 kPa under the condition of continuously filling hydrogen, heating the reaction chamber to 1000-1100 ℃ from a first preset temperature at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
In the specific implementation, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, step S8, after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen gas and argon gas which pass through the preheating pipeline into the reaction chamber, keeping the air pressure at a preset pressure, and continuously preserving the heat for a third preset time; the preheating pipeline is at a third preset temperature, and specifically comprises the following steps:
s80: after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen and argon gas which pass through a preheating pipeline into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1-3 h; wherein the temperature of the preheating pipeline is 200-300 ℃.
In specific implementation, in the method for cleaning fluorine ions and preparing an aluminide coating on a blade with a complex inner cavity, provided by the invention, in step S8, the flow rate of hydrogen chloride gas introduced into the reaction chamber can be controlled within a range of 0.5L/min to 1L/min, and the ratio of argon flow rate, hydrogen flow rate and hydrogen chloride gas flow rate can be 10: 10: 1, from which the flow rates of hydrogen and argon to the reaction chamber were also determined.
In the method for cleaning the complex inner cavity blade with fluoride ions and preparing the aluminide coating, the thickness of the aluminide coating is mainly controlled by the third preset time length of heat preservation in the chemical vapor deposition aluminizing process in the step S8, and the thickness of the aluminide coating can be controlled within the range of 20-50 microns.
In specific implementation, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, the pH value of the alkaline solution used in the steps S4 and S8 for treating the reacted tail gas is preferably 12-13, the alkaline solution with the pH value can avoid damage to a water ring pump or a pipeline due to excessive alkalinity, and meanwhile, a good absorption effect on acid gas in the tail gas can be ensured.
In specific implementation, in the method for cleaning the fluorine ions of the blades with the complex inner cavities and preparing the aluminide coating, the purities of hydrogen, argon, hydrogen fluoride and hydrogen chloride are all 99.9%, and the gas with high purity can be used for avoiding mixing other types of interference gas, so that the preparation of the coating is not influenced.
Example 2:
in the step S4 of the method for cleaning complex inner cavity blade with fluoride ions and preparing aluminide coating provided by the present invention, the gas for cleaning with fluoride ions continuously introduced into the reaction chamber is freon gas and hydrogen. The reason why freon gas is used instead of hydrogen fluoride gas is: the hydrogen fluoride gas has certain danger in the daily production process, and the Freon gas is used for replacing the hydrogen fluoride gas, so that the safety can be improved, and the effect of cleaning the fluorine ions can be still achieved.
In practical implementation, when step S1 in the method for cleaning fluorine ions and preparing an aluminide coating on a complicated inner-cavity blade provided by the invention is executed, 50g to 100g of aluminum blocks can be put into the graphite labyrinth in the reaction chamber. Specifically, the amount of the aluminum block to be put may be determined according to the length of the labyrinth passage of the graphite labyrinth.
In specific implementation, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, in step S3, the introduction of argon is stopped, hydrogen is continuously introduced into the reaction chamber, the pressure is kept at a preset pressure, the reaction chamber is heated from room temperature to a first preset temperature at a preset heating rate, and the temperature is kept for a first preset time, which specifically includes the following steps:
s30: stopping introducing the argon, continuously introducing the hydrogen into the reaction chamber, keeping the air pressure at 15-30 kPa, heating the reaction chamber from room temperature to 950-1000 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
In specific implementation, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, in step S4, after the heat preservation is finished, hydrogen and freon gas are continuously introduced into the reaction chamber, the air pressure is kept at a preset pressure, and the heat preservation is continuously carried out for a second preset time, which specifically includes the following steps:
s40: after the heat preservation is finished, continuously introducing hydrogen and Freon gas into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1 h.
In the method for cleaning the complex inner cavity blade by the fluoride ions and preparing the aluminide coating, in step S4, the flow rate of the freon gas introduced into the reaction chamber may be controlled within the range of 0.5L/min to 1L/min, and the ratio of the hydrogen flow rate to the freon gas flow rate may be 10: 1, whereby the flow rate of hydrogen to the reaction chamber can also be determined.
In the method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating, step S6 is to continuously fill hydrogen into the reaction chamber to discharge the residual freon gas out of the reaction chamber, so that the influence of the residual freon gas on the subsequent preparation of the aluminide coating can be avoided.
In a specific implementation, in the method for cleaning fluorine ions and preparing an aluminide coating on a blade with a complex inner cavity provided by the invention, in step S7, in a state of continuously filling hydrogen, the pressure is kept at a preset pressure, the reaction chamber is heated from the first preset temperature to the second preset temperature at a preset heating rate, and the temperature is kept for a first preset time, which specifically includes the following steps:
s70: keeping the air pressure at 15-30 kPa under the condition of continuously filling hydrogen, heating the reaction chamber to 1000-1100 ℃ from a first preset temperature at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
In the specific implementation, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, provided by the invention, step S8, after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen gas and argon gas which pass through the preheating pipeline into the reaction chamber, keeping the air pressure at a preset pressure, and continuously preserving the heat for a third preset time; the preheating pipeline is at a third preset temperature, and specifically comprises the following steps:
s80: after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen and argon gas which pass through a preheating pipeline into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1-3 h; wherein the temperature of the preheating pipeline is 200-300 ℃.
In specific implementation, in the method for cleaning fluorine ions and preparing an aluminide coating on a blade with a complex inner cavity, provided by the invention, in step S8, the flow rate of hydrogen chloride gas introduced into the reaction chamber can be controlled within a range of 0.5L/min to 1L/min, and the ratio of argon flow rate, hydrogen flow rate and hydrogen chloride gas flow rate can be 10: 10: 1, from which the flow rates of hydrogen and argon to the reaction chamber were also determined.
In the method for cleaning the complex inner cavity blade with fluoride ions and preparing the aluminide coating, the thickness of the aluminide coating is mainly controlled by the third preset time length of heat preservation in the chemical vapor deposition aluminizing process in the step S8, and the thickness of the aluminide coating can be controlled within the range of 20-50 microns.
In specific implementation, in the method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating, the pH value of the alkaline solution used in the steps S4 and S8 for treating the reacted tail gas is preferably 12-13, the alkaline solution with the pH value can avoid damage to a water ring pump or a pipeline due to excessive alkalinity, and meanwhile, a good absorption effect on acid gas in the tail gas can be ensured.
In specific implementation, in the method for cleaning the complex inner cavity blade by the fluoride ions and preparing the aluminide coating, the purities of hydrogen, argon, freon gas and hydrogen chloride gas are all 99.9%, and the gas with high purity can be used for avoiding mixing other types of interference gas, so that the preparation of the coating is not influenced.
Based on the same inventive concept, the invention also provides a device for cleaning the fluorine ions of the blades with complicated inner cavities and preparing the aluminide coating, as shown in fig. 3, the device comprises: the device comprises a reaction chamber 7, a graphite labyrinth 8, a blade tool 9, an aluminizing channel 10, a fluorine ion cleaning channel 11, a gas generation chamber 12, a thermocouple 13 and a metal mesh 14; wherein,
the graphite labyrinth 8 and the blade tool 9 are positioned in the reaction chamber 7, the blade tool 9 is used for installing a blade 15, the blade 15 is installed above the blade tool 9, and the blade tool 9 is positioned above the graphite labyrinth 8; the graphite labyrinth 8 is provided with a labyrinth passage, the labyrinth passage is used for placing an aluminum block, the air outlet of the labyrinth passage is aligned to a tenon 16 of a blade 15 arranged on the blade tool 9, the air inlet of the labyrinth passage is communicated with an aluminizing passage 10 positioned outside the reaction chamber 7, the gas generation chamber 12 is positioned on the aluminizing passage 10, the gas generation chamber 12 is used for placing the aluminum block, the aluminizing passage 10 is used for introducing hydrogen chloride gas, hydrogen gas and argon gas, and the gas in the aluminizing passage 10 passes through the gas generation chamber 12, then passes through the labyrinth passage and enters the blade 15 from the air outlet of the labyrinth passage;
the fluorine ion cleaning channel 11 is embedded into the aluminized channel 10 at a position between the gas generating chamber 12 and the inlet of the labyrinth channel, and penetrates from the center of the graphite labyrinth 8 to the outlet of the labyrinth channel; the fluorine ion cleaning channel 11 is used for introducing hydrogen fluoride gas, hydrogen and argon gas, or introducing Freon gas, hydrogen and argon gas;
the metal net 14 is positioned at the air outlet of the fluorine ion cleaning channel 11 and can be detached for cleaning, and the metal net 14 is used for preventing carbon generated by the reaction of the Freon gas and the hydrogen gas from entering the blade 15 at high temperature, so that the carbon generated by the reaction of the Freon gas and the hydrogen gas can be prevented from being deposited on the surface of the blade 15 at high temperature;
the bottom of the reaction chamber 7 is provided with an exhaust port 17 for discharging reaction off-gas.
It should be noted that, in the apparatus for cleaning fluorine ions and preparing an aluminide coating on a complex inner cavity blade according to the present invention, as for the example 1, in the case where the gas for cleaning fluorine ions continuously introduced into the reaction chamber is hydrogen fluoride gas and hydrogen gas when the step S4 in the method for cleaning fluorine ions and preparing an aluminide coating on a complex inner cavity blade according to the present invention is performed, the arrangement of the metal mesh may be omitted, as shown in fig. 4, because the hydrogen fluoride gas and the hydrogen gas do not react to generate carbon at a high temperature, and therefore, the metal mesh does not need to be arranged for filtering.
The device for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating can realize the cleaning of the fluorinion and the preparation of the aluminide coating. Specific examples of the fluoride ion cleaning process and the aluminide coating preparation process are described in detail below with reference to the apparatus shown in FIGS. 3 and 4, respectively.
Example 1 the fluorine ion cleaning process of the blade cavity is illustrated in connection with fig. 4. Firstly, cleaning and drying the deoiled and cleaned or surface sand-blasted blade 15, then assembling the cleaned and dried blade 15 with a blade tool 9, then placing the blade in a reaction chamber 7, and placing 50-100 g of aluminum blocks in a graphite labyrinth 8; then, a vacuum pump is used for vacuumizing, argon is introduced into the aluminizing channel 10 and the fluoride ion cleaning channel 11, the atmosphere in the reaction chamber 7 is repeatedly cleaned, and the gas is pumped away by the vacuum pump through an exhaust port 17; after the atmosphere in the reaction chamber 7 is cleaned, stopping introducing argon into the aluminizing channel 10 and the fluorine ion cleaning channel 11, introducing hydrogen into the reaction chamber 7 from the aluminizing channel 10, raising the temperature from room temperature to a first preset temperature of 950-1000 ℃ in an electric heating mode under the condition of keeping a preset pressure of 15-30 kPa, wherein the temperature raising rate is 10 ℃/min, monitoring the temperatures of different positions of the reaction chamber through thermocouples 13 at an upper position, a middle position and a lower position, and preserving the temperature for 1h after the first preset temperature is reached to ensure that the temperatures of the graphite labyrinth 8 and the blades 15 reach the first preset temperature; then, after the heat preservation is finished, continuously introducing high-purity hydrogen fluoride gas into the reaction chamber 7 from the fluorine ion cleaning channel 11, continuously introducing hydrogen gas into the reaction chamber 7 from the aluminizing channel 10, continuously preserving the heat for 1h under the condition that the preset pressure is kept at 15-30 kPa, enabling the hydrogen fluoride gas to pass through a central channel of the graphite labyrinth 8 instead of a labyrinth channel of the graphite labyrinth 8, and adopting large-flow gas to enable the fluorine ion cleaning atmosphere to enter an inner cavity of the blade 15 through an air inlet of a tenon 16 of the blade 15 during the period, so as to ensure that oxides on the surface of the inner cavity of the blade 15 fully react with the fluorine ion cleaning atmosphere, flow out of the air film cooling hole 4 and finally be discharged from an air outlet 17, and discharging tail gas into the atmosphere after passing through an alkaline solution pool; and finally, after the heat preservation is finished, stopping introducing the hydrogen fluoride gas, and finishing the cleaning of the fluorine ions in the inner cavity of the blade 15.
Example 2 the fluorine ion cleaning process of the blade cavity is illustrated in connection with fig. 3. Firstly, cleaning and drying the deoiled and cleaned or surface sand-blasted blade 15, then assembling the cleaned and dried blade 15 with a blade tool 9, then placing the blade in a reaction chamber 7, and placing 50-100 g of aluminum blocks in a graphite labyrinth 8; then, a vacuum pump is used for vacuumizing, argon is introduced into the aluminizing channel 10 and the fluoride ion cleaning channel 11, the atmosphere in the reaction chamber 7 is repeatedly cleaned, and the gas is pumped away by the vacuum pump through an exhaust port 17; after the atmosphere in the reaction chamber 7 is cleaned, stopping introducing argon into the aluminizing channel 10 and the fluorine ion cleaning channel 11, introducing hydrogen into the reaction chamber 7 from the aluminizing channel 10, raising the temperature from room temperature to a first preset temperature of 950-1000 ℃ in an electric heating mode under the condition of keeping a preset pressure of 15-30 kPa, wherein the temperature raising rate is 10 ℃/min, monitoring the temperatures of different positions of the reaction chamber through thermocouples 13 at an upper position, a middle position and a lower position, and preserving the temperature for 1h after the first preset temperature is reached to ensure that the temperatures of the graphite labyrinth 8 and the blades 15 reach the first preset temperature; then, after the heat preservation is finished, continuously introducing high-purity Freon gas and hydrogen into the reaction chamber 7 from the fluoride ion cleaning channel 11, continuously introducing the hydrogen gas into the reaction chamber 7 from the aluminizing channel 10, continuously preserving the heat for 1h under the condition of keeping the preset pressure of 15-30 kPa, wherein the Freon gas passes through a central channel of the graphite labyrinth 8 instead of the labyrinth channel of the graphite labyrinth 8, and during the period, a large-flow gas is adopted to ensure that the fluoride ion cleaning atmosphere enters an inner cavity of the blade 15 through an air inlet of a tenon 16 of the blade 15, so that oxides on the surface of the inner cavity of the blade 15 fully react with the fluoride ion cleaning atmosphere, flows out of the gas film cooling hole 4, is finally discharged from an air outlet 17, and tail gas is discharged into the atmosphere after passing through an alkaline solution pool; and finally, after the heat preservation is finished, stopping introducing the Freon gas, and finishing the cleaning of the fluorine ions in the inner cavity of the blade 15.
The process of preparing the aluminide coating on the surface and the inner cavity of the blade by chemical vapor deposition aluminizing is explained by combining the figure 3 and the figure 4. Firstly, filling hydrogen through an aluminizing channel 10 and a fluorine ion cleaning channel 11 to clean the atmosphere in the reaction chamber 7; then, under the condition of continuously filling hydrogen to keep the preset pressure of 15 kPa-30 kPa, heating the reaction chamber 7 from the first preset temperature to a second preset temperature of 1000-1100 ℃ in an electric heating mode, wherein the heating rate is 10 ℃/min, and keeping the temperature for 1h after the second preset temperature is reached to ensure that the graphite labyrinth 8 and the blades 15 reach the second preset temperature; then, after the heat preservation is finished, stopping filling hydrogen into the fluorine ion cleaning channel 11, continuously introducing hydrogen chloride gas, hydrogen and argon which pass through a preheating pipeline with the temperature of 300 ℃ into the reaction chamber 7 through the aluminizing channel 10, continuously preserving the heat for 1h to 3h under the condition of keeping the preset pressure of 15kPa to 30kPa, enabling the aluminizing atmosphere to pass through a labyrinth channel in which an aluminum block is placed in the graphite labyrinth 8 instead of a central channel of the graphite labyrinth 8, keeping the water ring pump to continuously work during the period, enabling the aluminizing atmosphere to fully flow through each structure of the blade 15, enter an inner cavity of the blade 15 through an air inlet of a tenon 16 of the blade 15 and flow out of an air film cooling hole 4, finally discharging the aluminizing atmosphere from an exhaust port 17, and discharging tail gas into the atmosphere after passing through an alkaline solution pool; and finally, after the heat preservation is finished, stopping introducing hydrogen chloride gas and hydrogen, keeping introducing argon gas from the aluminizing channel 10 to the blade 15, stopping vacuumizing after the blade 15 is cooled to the room temperature along with the reaction chamber 7, stopping introducing argon gas after the pressure of the reaction chamber 7 is increased to the atmospheric pressure, opening a bin, taking the blade 15, and finishing the preparation of the aluminide coating of the blade 15. The hydrogen and hydrogen chloride gas introduced into the aluminizing channel 10 react with the aluminum block in the gas generating chamber 12 at 200-300 ℃ to generate aluminum trichloride gas, the argon gas is used as a carrier gas to carry the aluminum trichloride to enter the graphite labyrinth 8, the aluminum trichloride further reacts with the aluminum block and the hydrogen in the graphite labyrinth 8 at 1000-1100 ℃ to generate aluminum dichloride and aluminum monochloride, the aluminum dichloride and the aluminum monochloride are pushed by the argon gas carrier gas to reach the surface and the outer surface of the cavity in the blade 15, and the aluminum dichloride with higher activity and the aluminum monochloride with high activity react with elements of the substrate (namely the surface and the outer surface of the inner cavity of the blade 15) to form an aluminizing coating.
According to the method and the device for cleaning the fluorine ions of the blade with the complex inner cavity and preparing the aluminide coating, the fluorine ions of the inner cavity of the blade are cleaned and the aluminide coating is prepared by a Chemical Vapor Deposition (CVD) method, and the fluorine ions of the inner cavity of the blade are cleaned to remove the residual oxide layer on the wall of the inner cavity, so that conditions are provided for preparing the aluminized coating by a subsequent chemical vapor deposition method. The two processes of fluoride ion cleaning and aluminide coating preparation are all completed by adopting CVD equipment, the CVD equipment does not need to be opened between the two processes, the blade does not need to be taken out, the two processes are integrally completed in the CVD equipment, the treatment time can be saved, the secondary pollution to the blade caused by taking out the blade midway can be avoided, the method is flexible and controllable, the prepared aluminide coating has high cleanliness, and the blade cannot be damaged. The method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating is particularly suitable for preparing the nickel-based single crystal superalloy guider blade with the complex inner cavity structure, the high-pressure turbine blade inner cavity and the surface high-temperature protective coating by a chemical vapor deposition method, and is also suitable for preparing the protective coatings of other high-temperature alloy parts.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A method for cleaning fluorine ions of a blade with a complex inner cavity and preparing an aluminide coating is characterized by comprising the following steps:
s1: placing the deoiled and cleaned or sand-blast cleaned blade in a reaction chamber of CVD equipment, and placing an aluminum block with preset quality in a graphite labyrinth in the reaction chamber;
s2: pumping the reaction chamber to a vacuum state, and then filling argon into the reaction chamber to atmospheric pressure to finish the primary cleaning of the blade; repeatedly cleaning for several times;
s3: stopping introducing argon, continuously introducing hydrogen into the reaction chamber, keeping the pressure at a preset pressure, heating the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and keeping the temperature for a first preset time;
s4: after the heat preservation is finished, continuously introducing hydrogen and hydrogen fluoride gas into the reaction chamber, or continuously introducing hydrogen and Freon gas into the reaction chamber, keeping the air pressure at a preset pressure, and continuously preserving the heat for a second preset time; hydrogen and hydrogen fluoride gas or hydrogen and Freon gas enter the cavity inside the blade through the air inlet of the blade tenon, flow out of the air film cooling hole, flow out of the air outlet of the reaction chamber, pass through the alkaline solution pool and then are discharged into the atmosphere;
s5: after the heat preservation is finished, stopping introducing hydrogen fluoride gas or Freon gas, and finishing the cleaning of the fluorine ions in the inner cavity of the blade;
s6: continuously filling hydrogen into the reaction chamber, and discharging residual hydrogen fluoride gas or Freon gas out of the reaction chamber;
s7: under the condition of continuously charging hydrogen, keeping the pressure at a preset pressure, heating the reaction chamber from the first preset temperature to a second preset temperature at a preset heating rate, and keeping the temperature for a first preset time;
s8: after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen and argon gas which pass through the preheating pipeline into the reaction chamber, keeping the pressure at a preset pressure, and continuously preserving the heat for a third preset time; wherein the temperature of the preheating pipeline is a third preset temperature; hydrogen chloride gas, hydrogen gas and argon gas enter the cavity inside the blade through the gas inlet of the blade tenon, flow out of the gas film cooling hole, flow out of the gas outlet of the reaction chamber, pass through the alkaline solution pool and then are discharged into the atmosphere;
s9: and after the heat preservation is finished, stopping introducing hydrogen chloride gas and hydrogen, continuously introducing argon, stopping vacuumizing after the blades are cooled to room temperature along with the reaction chamber, stopping introducing argon after the pressure of the reaction chamber is increased to the atmospheric pressure, opening the chamber, taking the blades, and finishing the preparation of the aluminide coating.
2. The method for cleaning the complex inner cavity blade with the fluoride ions and preparing the aluminide coating as claimed in claim 1, wherein step S3 comprises the following steps of stopping introducing the argon gas, continuously introducing the hydrogen gas into the reaction chamber, keeping the pressure at a preset pressure, heating the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and keeping the temperature for a first preset time, specifically:
s30: stopping introducing the argon, continuously introducing the hydrogen into the reaction chamber, keeping the air pressure at 15-30 kPa, heating the reaction chamber from room temperature to 950-1000 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
3. The method for cleaning the complex inner cavity blade by using the fluoride ions and preparing the aluminide coating, as claimed in claim 1, wherein in step S4, after the heat preservation is finished, hydrogen and hydrogen fluoride gas are continuously introduced into the reaction chamber, or hydrogen and freon gas are continuously introduced into the reaction chamber, so that the air pressure is kept at a preset pressure, and the heat preservation is continuously carried out for a second preset time, specifically comprising the following steps:
s40: after the heat preservation is finished, continuously introducing hydrogen and hydrogen fluoride gas into the reaction chamber, or continuously introducing hydrogen and Freon gas into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1 h.
4. The method for cleaning the complex-bore blade with fluoride ions and preparing the aluminide coating as claimed in claim 1, wherein the step S7 comprises the steps of maintaining the pressure at a predetermined pressure in a state of continuously charging hydrogen gas, heating the reaction chamber from the first predetermined temperature to a second predetermined temperature at a predetermined heating rate, and keeping the temperature for a first predetermined time, wherein the step S comprises the steps of:
s70: and under the condition of continuously filling hydrogen, keeping the air pressure at 15-30 kPa, heating the reaction chamber from the first preset temperature to 1000-1100 ℃ at the heating rate of 10 ℃/min, and preserving the heat for 1 h.
5. The method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating as claimed in claim 1, wherein in step S8, after the heat preservation is finished, the hydrogen chloride gas, the hydrogen gas and the argon gas which pass through the preheating pipeline are continuously introduced into the reaction chamber, the air pressure is kept at the preset pressure, and the heat preservation is continuously carried out for a third preset time; wherein, the temperature of preheating the pipeline is the third preset temperature, specifically includes the following steps:
s80: after the heat preservation is finished, continuously introducing hydrogen chloride gas, hydrogen and argon gas which pass through a preheating pipeline into the reaction chamber, keeping the air pressure at 15-30 kPa, and continuously preserving the heat for 1-3 h; wherein the temperature of the preheating pipeline is 200-300 ℃.
6. The method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating as claimed in claim 1, wherein the purity of the hydrogen gas, the argon gas and the hydrogen chloride gas is 99.9 percent, and the purity of the hydrogen fluoride gas or the freon gas is 99.9 percent.
7. The method for cleaning the fluorine ions of the blades with the complicated inner cavities and preparing the aluminide coating as claimed in claim 1, wherein the flow rate of hydrogen fluoride gas is 0.5L/min-1L/min, and the ratio of the flow rate of hydrogen to the flow rate of hydrogen fluoride gas is 10: 1; or,
the flow rate of the Freon gas is 0.5L/min-1L/min, the ratio of the hydrogen flow rate to the flow rate of the Freon gas is 10: 1.
8. the method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating as claimed in claim 1, wherein the flow rate of the hydrogen chloride gas is 0.5L/min to 1L/min;
the ratio of argon flow, hydrogen flow and hydrogen chloride gas flow is 10: 10: 1.
9. the method for cleaning the complex inner cavity blade by the fluorinion and preparing the aluminide coating as claimed in claim 1, wherein the thickness of the aluminide coating is 20-50 μm.
10. A device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings is characterized by comprising: the device comprises a reaction chamber, a graphite labyrinth, a blade tool, an aluminizing channel, a fluorine ion cleaning channel, a gas generation chamber, a thermocouple and a metal mesh; wherein,
the graphite labyrinth and the blade tool are positioned in the reaction chamber, the blade tool is used for installing a blade, the blade is installed above the blade tool, and the blade tool is positioned above the graphite labyrinth; the graphite labyrinth is provided with a labyrinth channel, the labyrinth channel is used for placing an aluminum block, the air outlet of the labyrinth channel is aligned to a tenon of a blade arranged on the blade tool, the air inlet of the labyrinth channel is communicated with an aluminizing channel positioned outside the reaction chamber, the gas generation chamber is positioned on the aluminizing channel, the gas generation chamber is used for placing the aluminum block, the aluminizing channel is used for introducing hydrogen chloride gas, hydrogen gas and argon gas, and the gas in the aluminizing channel passes through the gas generation chamber, then passes through the labyrinth channel and enters the blade from the air outlet of the labyrinth channel;
the fluorine ion cleaning channel is embedded into the aluminized channel at a position between the gas generating chamber and the inlet of the labyrinth channel and penetrates from the center of the graphite labyrinth to the outlet of the labyrinth channel; the fluorine ion cleaning channel is used for introducing hydrogen fluoride gas, hydrogen and argon, or introducing Freon gas, hydrogen and argon;
the metal net is positioned at the air outlet of the fluoride ion cleaning channel and used for preventing carbon generated by the reaction of Freon gas and hydrogen from entering the blade at high temperature;
the thermocouple is positioned on the inner wall of the reaction chamber and is used for measuring the temperature in the reaction chamber;
and an exhaust port for exhausting reaction tail gas is arranged at the bottom of the reaction chamber.
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