CN112430802B - 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
- Publication number
- CN112430802B CN112430802B CN202011071362.1A CN202011071362A CN112430802B CN 112430802 B CN112430802 B CN 112430802B CN 202011071362 A CN202011071362 A CN 202011071362A CN 112430802 B CN112430802 B CN 112430802B
- Authority
- CN
- China
- Prior art keywords
- gas
- hydrogen
- blade
- reaction chamber
- channel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Turbine Rotor Nozzle Sealing (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
本发明公开了一种复杂内腔叶片氟离子清洗及铝化物涂层制备的方法及装置,通过CVD对叶片内腔进行氟离子清洗和铝化物涂层制备,叶片内腔氟离子清洗的目的是去除内腔壁残留的氧化物层,为后续化学气相沉积法制备渗铝涂层提供条件。两个过程在CVD设备中一体化完成,无需打开CVD设备,无需取出叶片,不仅可以节约处理时间,还可以避免因中途取出叶片而对叶片造成二次污染,上述方法灵活可控,制备的铝化物涂层的清洁度高,且不会损伤叶片。上述方法尤其适用于具有复杂内腔结构的镍基单晶高温合金导向器叶片及高压涡轮叶片内腔及表面高温防护涂层的化学气相沉积法制备,同时也适用于其他高温合金零部件防护涂层的制备。
The invention discloses a method and device for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade. The blade inner cavity is cleaned by fluoride ion and aluminide coating is prepared by CVD. The purpose of fluoride ion cleaning in the blade inner cavity is as follows: The oxide layer remaining on the inner cavity wall is removed to provide conditions for the subsequent preparation of the aluminized coating by chemical vapor deposition. The two processes are integrated in the CVD equipment, and there is no need to open the CVD equipment or take out the blades, which not only saves processing time, but also avoids secondary pollution to the blades caused by taking out the blades in the middle. The above method is flexible and controllable, and the prepared aluminum The cleanliness of the chemical coating is high and does not damage the leaves. The above method is especially suitable for chemical vapor deposition of nickel-based single crystal superalloy guide vanes and high-pressure turbine blades with complex inner cavity structures for the preparation of high temperature protective coatings on the inner cavity and surface, and is also suitable for protective coatings for other superalloy parts. layer preparation.
Description
技术领域technical field
本发明涉及高温合金涂层及其制备技术领域,尤其涉及一种复杂内腔叶片氟离子清洗及铝化物涂层制备的方法及装置。The invention relates to the technical field of superalloy coatings and their preparation, in particular to a method and a device for fluoride ion cleaning of complex inner cavity blades and preparation of aluminide coatings.
背景技术Background technique
镍基高温单晶合金具有优良的高温力学性能,是目前制造先进飞机发动机和燃气轮机叶片的主要材料。由于发动机极其恶劣的工作环境,要求合金不仅要有良好的高温力学性能,还要有优异的抗高温氧化性能和抗热腐蚀性能。但在实际应用中,同一合金很难同时满足多种性能。为解决这一矛盾,最有效的方法是采用高温保护涂层技术。Nickel-based high temperature single crystal alloys have excellent high temperature mechanical properties and are currently the main materials for manufacturing advanced aircraft engines and gas turbine blades. Due to the extremely harsh working environment of the engine, the alloy is required not only to have good high temperature mechanical properties, but also to have excellent high temperature oxidation resistance and hot corrosion resistance. However, in practical applications, it is difficult for the same alloy to satisfy multiple properties at the same time. To solve this contradiction, the most effective way is to use high temperature protective coating technology.
在叶片生产过程中,在除去陶瓷模壳以及内腔脱除陶瓷型芯时,会分别在叶片外表面和内腔表面生成氧化物膜层,该氧化物膜层的存在将阻碍化学气相沉积渗铝过程中铝元素的内扩散,抑制铝化物涂层的形成。对叶片外表面进行喷砂清洗,可以得到清洁的金属表面,满足化学气相沉积渗铝前处理要求。公开号为CN104923520A的专利,提出磨粒流技术,利用磨料介质在压力下流动的最新机械加工工艺,对待加工的工件表面进行去毛刺、磨圆角等,可以减少表面波纹和粗糙度,达到精密加工的目的。对于具有简单内腔结构的叶片,可通过磨粒流技术对叶片内腔进行清洗。但对于具有复杂内腔结构的叶片(如双层壁结构),由于涡轮叶片的通道狭窄,孔隙小,无法对内腔彻底清洗,这会导致粘性磨料容易残留在其中,使得在内腔难以形成气相渗层,为清洗带来困难。In the blade production process, when the ceramic mold shell is removed and the ceramic core is removed from the inner cavity, an oxide film will be formed on the outer surface of the blade and the surface of the inner cavity respectively. The existence of the oxide film will hinder the chemical vapor deposition infiltration. The internal diffusion of aluminum elements in the aluminum process inhibits the formation of aluminide coatings. By blasting the outer surface of the blade, a clean metal surface can be obtained, which meets the requirements of chemical vapor deposition aluminizing pretreatment. The patent with publication number CN104923520A proposes abrasive flow technology, which uses the latest machining process of abrasive medium flowing under pressure to deburr and fillet the surface of the workpiece to be processed, which can reduce surface ripple and roughness and achieve precise processing purpose. For blades with a simple cavity structure, the inner cavity of the blade can be cleaned by abrasive flow technology. However, for blades with complex inner cavity structure (such as double-walled structure), due to the narrow channel and small pores of the turbine blade, the inner cavity cannot be thoroughly cleaned, which will cause the viscous abrasive to remain in it, making it difficult to form the inner cavity. The vapor infiltration layer makes cleaning difficult.
目前常见使用的渗铝方法主要有:包埋渗铝、气相渗铝(VPA)和化学气相沉积法渗铝(CVD)。包埋渗铝的缺点是包埋粉末在高温时易于烧结,堵塞冷却孔,渗铝时很难准确导入叶片的微小通道内,在内腔中难以制备出理想的防护涂层。气相渗铝的缺点是虽然实现了分离粉末与渗件,但参数控制存在局限性。CVD渗铝可以对叶片中具有复杂结构的内腔进行渗铝,并且不需要粉末,在一定温度和压强下同时控制气体流量就可以控制涂层的生长速率、结构和性能。因此,CVD渗铝是三种工艺中最洁净的工艺,是目前应用最广泛的工艺。At present, the commonly used aluminizing methods mainly include embedded aluminizing, vapor-phase aluminizing (VPA) and chemical vapor deposition (CVD). The disadvantage of embedded aluminizing is that the embedded powder is easy to sinter at high temperature, blocking the cooling holes, and it is difficult to accurately guide the micro-channel of the blade during aluminizing, and it is difficult to prepare an ideal protective coating in the inner cavity. The disadvantage of gas-phase aluminizing is that although the separation of powder and infiltrated parts is achieved, there are limitations in parameter control. CVD aluminizing can aluminize the inner cavity with complex structure in the blade, and does not require powder, and the growth rate, structure and performance of the coating can be controlled by simultaneously controlling the gas flow under a certain temperature and pressure. Therefore, CVD aluminizing is the cleanest process among the three processes, and is currently the most widely used process.
公开号为CN105695929A的专利公开了一种适用于高Mo含量复杂内腔结构叶片防护涂层的制备方法,该制备方法为采用马弗炉进行叶片内腔氟离子清洗及气相渗铝硅涂层的制备,这种方法的缺点是中途需要将叶片从马弗炉中取出重新处理一下,加入固体渗剂,清洗和涂层制备不能做到一体化处理,需要对马弗炉进行多次升温、降温,增加了整个处理过程的时间。The patent publication number CN105695929A discloses a preparation method suitable for a protective coating of a blade with a high Mo content and a complex inner cavity structure. The disadvantage of this method is that the blade needs to be taken out of the muffle furnace for reprocessing, and a solid penetration agent is added. The cleaning and coating preparation cannot be integrated, and the muffle furnace needs to be heated and cooled several times. , which increases the overall processing time.
发明内容SUMMARY OF THE INVENTION
有鉴于此,本发明提供了一种复杂内腔叶片氟离子清洗及铝化物涂层制备的方法及装置,用以实现一体化完成复杂内腔叶片的氧化膜层清洗处理和铝化物防护涂层的制备。In view of this, the present invention provides a method and device for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades, so as to realize the integrated completion of oxide film layer cleaning treatment and aluminide protective coating of complex inner cavity blades preparation.
本发明提供的一种复杂内腔叶片氟离子清洗及铝化物涂层制备的方法,包括如下步骤:The invention provides a method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade, comprising the following steps:
S1:将去油清洗或喷砂清洗后的叶片置于CVD设备的反应室中,并在反应室内的石墨迷宫中放入预设质量的铝块;S1: place the blade after degreasing cleaning or sandblast cleaning in the reaction chamber of the CVD equipment, and put aluminum blocks of preset quality into the graphite labyrinth in the reaction chamber;
S2:将反应室抽至真空状态后,向反应室充入氩气至大气压,完成对叶片的一次清洗;反复清洗若干次;S2: After the reaction chamber is evacuated to a vacuum state, the reaction chamber is filled with argon to atmospheric pressure to complete one cleaning of the blades; repeated cleaning several times;
S3:停止通入氩气,向反应室持续充入氢气,气压保持预设压强,将反应室从室温以预设升温速率加热至第一预设温度,并保温第一预设时长;S3: stop feeding argon gas, continuously fill the reaction chamber with hydrogen gas, keep the air pressure at a preset pressure, heat the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and maintain the temperature for a first preset time period;
S4:保温结束后,向反应室持续通入氢气和氟化氢气体,或者向反应室持续通入氢气和氟利昂气体,使气压保持预设压强,继续保温第二预设时长;其中,氢气和氟化氢气体,或者氢气和氟利昂气体,经叶片榫头进气口进入叶片内部空腔并由气膜冷却孔流出,再由反应室出气口流出后通过碱性溶液池后排入大气;S4: After the heat preservation is completed, hydrogen and hydrogen fluoride gas are continuously introduced into the reaction chamber, or hydrogen and freon gas are continuously introduced into the reaction chamber to keep the air pressure at the preset pressure, and the heat preservation is continued for a second preset time period; wherein, the hydrogen and hydrogen fluoride gases are , or hydrogen and freon gas, enter the inner cavity of the blade through the air inlet of the tenon of the blade and flow out from the air film cooling hole, and then flow out from the outlet of the reaction chamber and then pass through the alkaline solution pool and then discharge into the atmosphere;
S5:保温结束后,停止通入氟化氢气体或氟利昂气体,完成对叶片内腔的氟离子清洗;S5: After the heat preservation is over, stop feeding hydrogen fluoride gas or freon gas to complete the cleaning of fluoride ions in the inner cavity of the blade;
S6:向反应室持续充入氢气,使残留的氟化氢气体或氟利昂气体排出反应室;S6: continue to fill the reaction chamber with hydrogen, so that the residual hydrogen fluoride gas or freon gas is discharged from the reaction chamber;
S7:在持续充入氢气的状态下,气压保持预设压强,将反应室从所述第一预设温度以预设升温速率加热至第二预设温度,并保温第一预设时长;S7: in the state of being continuously charged with hydrogen, the air pressure is maintained at a preset pressure, and the reaction chamber is heated from the first preset temperature to a second preset temperature at a preset heating rate, and maintained for a first preset time period;
S8:保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持预设压强,继续保温第三预设时长;其中,预热管道的温度为第三预设温度;氯化氢气体、氢气和氩气经叶片榫头进气口进入叶片内部空腔并由气膜冷却孔流出,再由反应室出气口流出后通过碱性溶液池后排入大气;S8: After the heat preservation is completed, the hydrogen chloride gas, hydrogen gas and argon gas passing through the preheating pipeline are continuously fed into the reaction chamber, the air pressure is maintained at the preset pressure, and the heat preservation is continued for a third preset time period; wherein, the temperature of the preheating pipeline is the third preheating pipeline. Set the temperature; hydrogen chloride gas, hydrogen gas and argon gas enter the inner cavity of the blade through the air inlet of the tenon of the blade and flow out from the air film cooling hole, and then flow out from the outlet of the reaction chamber and then pass through the alkaline solution pool and then discharge into the atmosphere;
S9:保温结束后,停止通入氯化氢气体和氢气,持续通入氩气,待叶片随反应室冷却至室温后,停止抽真空,待反应室压强升至大气压后,停止通入氩气,开仓取叶片,完成铝化物涂层的制备。S9: After the heat preservation is completed, stop feeding hydrogen chloride gas and hydrogen gas, and continue feeding argon gas. After the blade is cooled to room temperature with the reaction chamber, stop vacuuming. After the pressure in the reaction chamber rises to atmospheric pressure, stop feeding argon gas and turn on The leaves are taken out and the preparation of the aluminide coating is completed.
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S3,停止通入氩气,向反应室持续充入氢气,气压保持预设压强,将反应室从室温以预设升温速率加热至第一预设温度,并保温第一预设时长,具体包括如下步骤:In a possible implementation manner, in the above-mentioned method for fluorine ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, step S3, stopping the introduction of argon gas, continuously filling the reaction chamber with hydrogen gas, and the pressure Maintaining the preset pressure, heating the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and maintaining the temperature for a first preset time period, specifically including the following steps:
S30:停止通入氩气,向反应室持续充入氢气,气压保持15kPa~30kPa,将反应室从室温以10℃/min的升温速率加热至950℃~1000℃,并保温1h。S30: Stop feeding argon gas, continue to charge hydrogen into the reaction chamber, keep the air pressure at 15kPa to 30kPa, heat the reaction chamber from room temperature to 950°C to 1000°C at a heating rate of 10°C/min, and keep the temperature for 1 hour.
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S4,保温结束后,向反应室持续通入氢气和氟化氢气体,或者向反应室持续通入氢气和氟利昂气体,使气压保持预设压强,继续保温第二预设时长,具体包括如下步骤:In a possible implementation manner, in the above-mentioned method for fluorine ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, in step S4, after the heat preservation is completed, hydrogen and hydrogen fluoride gas are continuously introduced into the reaction chamber, Or continuously feed hydrogen and freon gas into the reaction chamber, keep the air pressure at a preset pressure, and continue to keep the temperature for a second preset time, which specifically includes the following steps:
S40:保温结束后,向反应室持续通入氢气和氟化氢气体,或者向反应室持续通入氢气和氟利昂气体,使气压保持15kPa~30kPa,继续保温1h。S40: After the heat preservation is completed, 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 maintained at 15kPa to 30kPa, and the heat preservation is continued for 1 hour.
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S7,在持续充入氢气的状态下,气压保持预设压强,将反应室从所述第一预设温度以预设升温速率加热至第二预设温度,并保温第一预设时长,具体包括如下步骤:In a possible implementation manner, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, in step S7, the air pressure is maintained at a preset pressure in the state of continuous filling of hydrogen gas, Heating the reaction chamber from the first preset temperature to a second preset temperature at a preset heating rate, and maintaining the temperature for a first preset time period, specifically includes the following steps:
S70:在持续充入氢气的状态下,气压保持15kPa~30kPa,将反应室从所述第一预设温度以10℃/min的升温速率加热至1000℃~1100℃,并保温1h。S70: Under the state of continuous charging of hydrogen, the air pressure is maintained at 15kPa~30kPa, and the reaction chamber is heated from the first preset temperature to 1000°C~1100°C at a heating rate of 10°C/min, and kept for 1 hour.
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S8,保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持预设压强,继续保温第三预设时长;其中,预热管道的温度为第三预设温度,具体包括如下步骤:In a possible implementation manner, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, in step S8, after the heat preservation is completed, the reaction chamber is continuously fed into the reaction chamber through the preheating pipeline. Hydrogen chloride gas, hydrogen gas and argon gas, the air pressure is maintained at the preset pressure, and the temperature is kept for a third preset time period; wherein, the temperature of the preheating pipeline is the third preset temperature, which specifically includes the following steps:
S80:保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持15kPa~30kPa,继续保温1h~3h;其中,预热管道的温度为200℃~300℃。S80: After the heat preservation is completed, the hydrogen chloride gas, hydrogen gas and argon gas passing through the preheating pipeline are continuously introduced into the reaction chamber, the pressure is maintained at 15kPa~30kPa, and the heat preservation is continued for 1h~3h; wherein, the temperature of the preheating pipeline is 200℃~300℃ .
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,氢气、氩气以及氯化氢气体的纯度均为99.9%,氟化氢气体或氟利昂气体的纯度为99.9%。In a possible implementation manner, in the above-mentioned method for fluorine ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, the purity of hydrogen gas, argon gas and hydrogen chloride gas are all 99.9%, and the purity of hydrogen fluoride gas or Freon gas is 99.9%. The purity of the gas is 99.9%.
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,氟化氢气体流量为0.5L/min~1L/min,氢气流量与氟化氢气体流量的比例为10:1;或者,In a possible implementation manner, in the above-mentioned method for fluorine ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, the flow rate of hydrogen fluoride gas is 0.5L/min~1L/min, and the flow rate of hydrogen gas is the same as that of hydrogen fluoride gas. The ratio of flow is 10:1; or,
氟利昂气体流量为0.5L/min~1L/min,氢气流量与氟利昂气体流量的比例为10:1。The freon gas flow is 0.5L/min~1L/min, and the ratio of hydrogen flow to freon gas flow is 10:1.
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,氯化氢气体流量为0.5L/min~1L/min;In a possible implementation manner, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, the flow rate of hydrogen chloride gas is 0.5L/min~1L/min;
氩气流量、氢气流量和氯化氢气体流量的比例为10:10:1。The ratio of argon flow, hydrogen flow and hydrogen chloride gas flow is 10:10:1.
在一种可能的实现方式中,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,铝化物涂层的厚度为20μm~50μm。In a possible implementation manner, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, the thickness of the aluminide coating is 20 μm˜50 μm.
本发明还提供了一种复杂内腔叶片氟离子清洗及铝化物涂层制备的装置,包括:反应室、石墨迷宫、叶片工装、渗铝通道、氟离子清洗通道、气体产生室、热电偶及金属网;其中,The invention also provides a device for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade, comprising: a reaction chamber, a graphite labyrinth, a blade tooling, an aluminizing channel, a fluoride ion cleaning channel, a gas generating chamber, a thermocouple and metal mesh; of which,
所述石墨迷宫和所述叶片工装位于所述反应室内,所述叶片工装用于安装叶片,叶片安装于所述叶片工装的上方,所述叶片工装位于所述石墨迷宫的上方;所述石墨迷宫具有迷宫通道,所述迷宫通道用于放置铝块,所述迷宫通道的出气口对准安装于所述叶片工装上的叶片的榫头,所述迷宫通道的进气口与位于所述反应室外的渗铝通道连通,所述气体产生室位于所述渗铝通道上,所述气体产生室用于放置铝块,所述渗铝通道用于通入氯化氢气体、氢气和氩气,所述渗铝通道内的气体经过所述气体产生室后经过所述迷宫通道,从所述迷宫通道的出气口进入叶片;The graphite labyrinth and the blade tooling are located in the reaction chamber, the blade tooling is used for installing a blade, the blade is installed above the blade tooling, and the blade tooling is located above the graphite labyrinth; the graphite labyrinth There is a labyrinth channel, the labyrinth channel is used to place the aluminum block, the air outlet of the labyrinth channel is aligned with the tenon of the blade installed on the blade tool, and the air inlet of the labyrinth channel is located outside the reaction chamber. The aluminizing channel is connected, the gas generating chamber is located on the aluminizing channel, the gas generating 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 aluminizing channel is The gas in the channel passes through the labyrinth channel after passing through the gas generating chamber, and enters the blade from the air outlet of the labyrinth channel;
所述氟离子清洗通道在所述气体产生室与所述迷宫通道进气口之间的位置嵌套进所述渗铝通道内,从所述石墨迷宫的中心穿过直至所述迷宫通道的出气口处;所述氟离子清洗通道用于通入氟化氢气体、氢气和氩气,或者通入氟利昂气体、氢气和氩气;The fluoride ion cleaning channel is nested into the aluminizing channel at the position between the gas generating chamber and the inlet of the labyrinth channel, and passes through the center of the graphite labyrinth until the outlet of the labyrinth channel. At the gas port; the fluoride ion cleaning channel is used for feeding hydrogen fluoride gas, hydrogen gas and argon gas, or feeding Freon gas, hydrogen gas and argon gas;
所述金属网位于所述氟离子清洗通道的出气口处,用于阻挡在高温时氟利昂气体与氢气反应生成的碳进入叶片;The metal mesh is located at the air outlet of the fluoride ion cleaning channel, and is used to prevent the carbon generated by the reaction of the Freon gas and the hydrogen from entering the blade at a high temperature;
所述热电偶位于所述反应室的内壁上,用于对反应室内的温度进行测量;The thermocouple is located on the inner wall of the reaction chamber for measuring the temperature in the reaction chamber;
所述反应室的底部设有用于排出反应尾气的排气口。The bottom of the reaction chamber is provided with an exhaust port for discharging reaction exhaust gas.
本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法及装置,通过化学气相沉积法(CVD)对叶片内腔进行氟离子清洗和铝化物涂层制备,叶片内腔氟离子清洗的目的是去除内腔壁残留的氧化物层,为后续化学气相沉积法制备渗铝涂层提供条件。氟离子清洗和铝化物涂层制备这两个过程都是采用CVD设备完成,并且这两个过程之间无需打开CVD设备,无需取出叶片,两个过程在CVD设备中一体化完成,不仅可以节约处理时间,还可以避免因中途取出叶片而对叶片造成二次污染,上述方法灵活可控,制备的铝化物涂层的清洁度高,且不会损伤叶片。本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法,尤其适用于具有复杂内腔结构的镍基单晶高温合金导向器叶片及高压涡轮叶片内腔及表面高温防护涂层的化学气相沉积法制备,同时也适用于其他高温合金零部件防护涂层的制备。The method and device for fluoride ion cleaning and aluminide coating preparation of the above-mentioned complex inner cavity blade provided by the present invention, the blade inner cavity is cleaned by fluoride ion and aluminide coating is prepared by chemical vapor deposition (CVD), and the blade inner cavity fluorine The purpose of ion cleaning is to remove the residual oxide layer on the inner cavity wall and provide conditions for the subsequent preparation of aluminized coating by chemical vapor deposition. The two processes of fluoride ion cleaning and aluminide coating preparation are both completed by CVD equipment, and there is no need to open the CVD equipment or take out the blades between the two processes. The two processes are integrated in the CVD equipment, which not only saves money The processing time can also avoid secondary pollution of the leaves due to the removal of the leaves in the middle. The above method is flexible and controllable, and the prepared aluminide coating has high cleanliness and will not damage the leaves. The method for fluoride ion cleaning and aluminide coating preparation of the above-mentioned complex inner cavity blade provided by the present invention is especially suitable for nickel-based single crystal superalloy guide blades with complex inner cavity structure and high-pressure turbine blade inner cavity and surface high temperature protective coating It is also suitable for the preparation of protective coatings for other superalloy parts.
附图说明Description of drawings
图1为本发明提供的一种复杂内腔叶片氟离子清洗及铝化物涂层制备的方法的流程图;1 is a flow chart of a method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention;
图2为一种具有复杂内腔结构的叶片的剖面图;Figure 2 is a cross-sectional view of a blade with a complex cavity structure;
图3为本发明提供的一种复杂内腔叶片氟离子清洗及铝化物涂层制备的装置的结构示意图之一;3 is one of the structural schematic diagrams of a device for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention;
图4为本发明提供的一种复杂内腔叶片氟离子清洗及铝化物涂层制备的装置的结构示意图之二。FIG. 4 is a second schematic structural diagram of a device for cleaning fluoride ions and preparing aluminide coating for a complex inner cavity blade provided by the present invention.
附图说明:内壁1,冲击冷却孔2,外壁3,气膜冷却孔4,中间夹层5,叶片内部6,反应室7,石墨迷宫8,叶片工装9,渗铝通道10,氟离子清洗通道11,气体产生室12,热电偶13,金属网14,叶片15,榫头16,排气口17。Description of drawings: inner wall 1, impact cooling hole 2, outer wall 3, gas film cooling hole 4,
具体实施方式Detailed ways
下面将结合本发明实施方式中的附图,对本发明实施方式中的技术方案进行清楚、完整的描述,显然,所描述的实施方式仅仅是作为例示,并非用于限制本发明。The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are merely illustrative and not intended to limit the present invention.
本发明提供的一种复杂内腔叶片氟离子清洗及铝化物涂层制备的方法,如图1所示,包括如下步骤:A method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, as shown in FIG. 1 , includes the following steps:
S1:将去油清洗或喷砂清洗后的叶片置于CVD设备的反应室中,并在反应室内的石墨迷宫中放入预设质量的铝块;S1: place the blade after degreasing cleaning or sandblast cleaning in the reaction chamber of the CVD equipment, and put aluminum blocks of preset quality into the graphite labyrinth in the reaction chamber;
S2:将反应室抽至真空状态后,向反应室充入氩气至大气压,完成对叶片的一次清洗;反复清洗若干次;S2: After the reaction chamber is evacuated to a vacuum state, the reaction chamber is filled with argon to atmospheric pressure to complete one cleaning of the blades; repeated cleaning several times;
S3:停止通入氩气,向反应室持续充入氢气,气压保持预设压强,将反应室从室温以预设升温速率加热至第一预设温度,并保温第一预设时长;S3: stop feeding argon gas, continuously fill the reaction chamber with hydrogen gas, keep the air pressure at a preset pressure, heat the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and maintain the temperature for a first preset time period;
S4:保温结束后,向反应室持续通入氢气和氟化氢气体,或者向反应室持续通入氢气和氟利昂气体,使气压保持预设压强,继续保温第二预设时长;其中,氢气和氟化氢气体,或者氢气和氟利昂气体,经叶片榫头进气口进入叶片内部空腔并由气膜冷却孔流出,再由反应室出气口流出后通过碱性溶液池后排入大气;S4: After the heat preservation is completed, hydrogen and hydrogen fluoride gas are continuously introduced into the reaction chamber, or hydrogen and freon gas are continuously introduced into the reaction chamber to keep the air pressure at the preset pressure, and the heat preservation is continued for a second preset time period; wherein, the hydrogen and hydrogen fluoride gases are , or hydrogen and freon gas, enter the inner cavity of the blade through the air inlet of the tenon of the blade and flow out from the air film cooling hole, and then flow out from the outlet of the reaction chamber and then pass through the alkaline solution pool and then discharge into the atmosphere;
S5:保温结束后,停止通入氟化氢气体或氟利昂气体,完成对叶片内腔的氟离子清洗;S5: After the heat preservation is over, stop feeding hydrogen fluoride gas or freon gas to complete the cleaning of fluoride ions in the inner cavity of the blade;
S6:向反应室持续充入氢气,使残留的氟化氢气体或氟利昂气体排出反应室;S6: continue to fill the reaction chamber with hydrogen, so that the residual hydrogen fluoride gas or freon gas is discharged from the reaction chamber;
S7:在持续充入氢气的状态下,气压保持预设压强,将反应室从第一预设温度以预设升温速率加热至第二预设温度,并保温第一预设时长;S7: in the state of being continuously charged with hydrogen, the air pressure is maintained at the preset pressure, the reaction chamber is heated from the first preset temperature to the second preset temperature at the preset heating rate, and the temperature is maintained for the first preset time period;
S8:保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持预设压强,继续保温第三预设时长;其中,预热管道的温度为第三预设温度;氯化氢气体、氢气和氩气经叶片榫头进气口进入叶片内部空腔并由气膜冷却孔流出,再由反应室出气口流出后通过碱性溶液池后排入大气;S8: After the heat preservation is completed, the hydrogen chloride gas, hydrogen gas and argon gas passing through the preheating pipeline are continuously fed into the reaction chamber, the air pressure is maintained at the preset pressure, and the heat preservation is continued for a third preset time period; wherein, the temperature of the preheating pipeline is the third preheating pipeline. Set the temperature; hydrogen chloride gas, hydrogen gas and argon gas enter the inner cavity of the blade through the air inlet of the tenon of the blade and flow out from the air film cooling hole, and then flow out from the outlet of the reaction chamber and then pass through the alkaline solution pool and then discharge into the atmosphere;
S9:保温结束后,停止通入氯化氢气体和氢气,持续通入氩气,待叶片随反应室冷却至室温后,停止抽真空,待反应室压强升至大气压后,停止通入氩气,开仓取叶片,完成铝化物涂层的制备。S9: After the heat preservation is completed, stop feeding hydrogen chloride gas and hydrogen gas, and continue feeding argon gas. After the blade is cooled to room temperature with the reaction chamber, stop vacuuming. After the pressure in the reaction chamber rises to atmospheric pressure, stop feeding argon gas and turn on The leaves are taken out and the preparation of the aluminide coating is completed.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S1~S5为通过化学气相沉积法(CVD)对叶片内腔的氟离子清洗过程,叶片内腔氟离子清洗的目的是去除内腔壁残留的氧化物层,为后续化学气相沉积法制备渗铝涂层提供条件。步骤S6~S9为通过化学气相沉积法渗铝来制备叶片内腔的铝化物涂层的过程。上述两个过程都是采用CVD设备完成,并且两个过程之间无需打开CVD设备,无需取出叶片,两个过程在CVD设备中一体化完成,不仅可以节约处理时间,还可以避免因中途取出叶片而对叶片造成二次污染,上述方法灵活可控,制备的铝化物涂层的清洁度高,且不会损伤叶片。本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法,尤其适用于具有复杂内腔结构的镍基单晶高温合金导向器叶片及高压涡轮叶片内腔及表面高温防护涂层的化学气相沉积法制备,同时也适用于其他高温合金零部件防护涂层的制备。In the specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, steps S1 to S5 are the fluoride ion cleaning process of the blade inner cavity by chemical vapor deposition (CVD). , The purpose of fluoride ion cleaning in the inner cavity of the blade is to remove the residual oxide layer on the inner cavity wall and provide conditions for the subsequent chemical vapor deposition method to prepare the aluminized coating. Steps S6 to S9 are a process of preparing the aluminide coating of the inner cavity of the blade by chemical vapor deposition aluminizing. The above two processes are completed by CVD equipment, and there is no need to open the CVD equipment or take out the blades between the two processes. The two processes are integrated in the CVD equipment, which not only saves the processing time, but also avoids taking out the blades midway. As for secondary pollution to the blade, the above method is flexible and controllable, the prepared aluminide coating has high cleanliness and will not damage the blade. The method for fluoride ion cleaning and aluminide coating preparation of the above-mentioned complex inner cavity blade provided by the present invention is especially suitable for nickel-based single crystal superalloy guide blades with complex inner cavity structure and high-pressure turbine blade inner cavity and surface high temperature protective coating It is also suitable for the preparation of protective coatings for other superalloy parts.
图2为一种具有复杂内腔结构的叶片的剖面图。与普通空心叶片不同,复杂内腔叶片为双层壁,内壁1通过铸造加工形成多个冲击冷却孔2,外壁3通过电火花加工形成多个气膜冷却孔4,中间夹层5厚度约为1mm。由于该类叶片的复杂结构,使得内腔表面的氧化物无法用磨料流等加工方法去除,并且磨料介质难以清洗,这给后续内腔化学气相沉积渗层制备带来困难。本发明通过采用氟离子清洗对叶片内腔表面进行清洗,去除氧化物膜层,为后续化学气相沉积法制备铝化物涂层提供条件。叶片内腔氟离子清洗通过特定的工装设计实现(具体可以参见后面的装置部分),使氟离子清洗气氛通过导向器叶片两端盖板或涡轮叶片榫头处进入叶片内部6,并依次通过冲击冷却孔2和中间夹层5,由气膜冷却孔4排出。在高温950℃~1000℃条件下,氟离子清洗气氛与氧化物层发生反应,形成气相产物,实现叶片内腔(叶片内部6及中间夹层5)的氟离子清洗。具体地,通入的氟化氢气体会与叶片内腔附着的氧化物(主要是铝、钛、铬氧化物及其复合氧化物)充分反应,反应式如下:Figure 2 is a cross-sectional view of a blade with a complex cavity structure. Different from ordinary hollow blades, the complex inner cavity blade is double-walled. The inner wall 1 is formed by casting to form a plurality of impact cooling holes 2, and the outer wall 3 is formed by EDM to form a plurality of film cooling holes 4. The thickness of the
6HF+Al2O3→2AlF3+3H2O6HF+Al 2 O 3 →2AlF 3 +3H 2 O
4HF+TiO2→TiF4+2H2O4HF+TiO 2 →TiF 4 +2H 2 O
6HF+Cr2O3→2CrF3+F2+3H2O。6HF + Cr2O3 → 2CrF3 +F2+ 3H2O .
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,对于铝化物涂层的制备过程,在基底(即叶片内腔表面和外表面)为镍基高温合金时,铝化物涂层的最外层/表层为β-NiAl相,表层与基底之间为互扩散区。在高温环境下,NiAl相会被氧化,从而在铝化物涂层表层相的表面形成一层致密的氧化铝,可以提高叶片的高温抗氧化性。在利用化学气相沉积法渗铝制备铝化物涂层后,还可以在铝化物涂层表面进一步制备MCrAlY包覆涂层及陶瓷基热障涂层。In the specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, for the preparation process of the aluminide coating, the substrate (ie, the inner cavity surface and the outer surface of the blade) is as follows: In nickel-based superalloys, the outermost/surface layer of the aluminide coating is β-NiAl phase, and the interdiffusion zone is between the surface layer and the substrate. In a high temperature environment, the NiAl phase will be oxidized, thereby forming a dense layer of alumina on the surface of the surface phase of the aluminide coating, which can improve the high temperature oxidation resistance of the blade. After the aluminide coating is prepared by chemical vapor deposition, the MCrAlY cladding coating and the ceramic-based thermal barrier coating can be further prepared on the surface of the aluminide coating.
下面通过两个具体的实施例对本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法在具体实施例中的具体参数和具体条件进行详细说明。The specific parameters and specific conditions in the specific embodiments of the method for fluoride ion cleaning and aluminide coating preparation of the complex inner cavity blade provided by the present invention are described in detail below through two specific embodiments.
实施例1:Example 1:
在执行本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中的步骤S4时,向反应室持续通入的用于氟离子清洗的气体为氟化氢气体和氢气。When performing step S4 in the method for fluoride ion cleaning and aluminide coating preparation of the complex inner cavity blade provided by the present invention, the gases continuously fed into the reaction chamber for fluoride ion cleaning are hydrogen fluoride gas and hydrogen gas.
在具体实施时,在执行本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中的步骤S1时,可以在反应室内的石墨迷宫中放入50g~100g的铝块。具体地,铝块的投放量可以根据石墨迷宫的迷宫通道的长度来确定。In specific implementation, when performing step S1 in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, 50g-100g aluminum blocks may be placed in the graphite labyrinth in the reaction chamber. Specifically, the throwing amount of the aluminum block can be determined according to the length of the labyrinth channel of the graphite labyrinth.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S3,停止通入氩气,向反应室持续充入氢气,气压保持预设压强,将反应室从室温以预设升温速率加热至第一预设温度,并保温第一预设时长,具体可以包括如下步骤:In specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating for complex inner cavity blades provided by the present invention, in step S3, the supply of argon gas is stopped, and hydrogen gas is continuously filled into the reaction chamber, and the gas pressure is maintained at a preset pressure , heating the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and maintaining the temperature for a first preset time period, which may specifically include the following steps:
S30:停止通入氩气,向反应室持续充入氢气,气压保持15kPa~30kPa,将反应室从室温以10℃/min的升温速率加热至950℃~1000℃,并保温1h。S30: Stop feeding argon gas, continue to charge hydrogen into the reaction chamber, keep the air pressure at 15kPa to 30kPa, heat the reaction chamber from room temperature to 950°C to 1000°C at a heating rate of 10°C/min, and keep the temperature for 1 hour.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S4,保温结束后,向反应室持续通入氢气和氟化氢气体,气压保持预设压强,继续保温第二预设时长,具体可以包括如下步骤:In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, in step S4, after the heat preservation is completed, hydrogen and hydrogen fluoride gas are continuously introduced into the reaction chamber, and the gas pressure is maintained at a preset value pressure, and continue to keep warm for a second preset time period, which may specifically include the following steps:
S40:保温结束后,向反应室持续通入氢气和氟化氢气体,气压保持15kPa~30kPa,继续保温1h。S40: After the heat preservation is completed, hydrogen and hydrogen fluoride gas are continuously introduced into the reaction chamber, the air pressure is maintained at 15 kPa to 30 kPa, and the heat preservation is continued for 1 hour.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S4中,向反应室通入的氟化氢气体的流量可以控制在0.5L/min~1L/min范围,氢气流量与氟化氢气体流量的比例可以为10:1,由此,向反应室通入的氢气的流量也可以确定。In specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing an aluminide coating for a complex inner cavity blade provided by the present invention, in step S4, the flow rate of the hydrogen fluoride gas introduced into the reaction chamber can be controlled at 0.5L/min~ In the range of 1 L/min, the ratio of the hydrogen flow to the hydrogen fluoride gas flow can be 10:1, and thus, the flow rate of the hydrogen gas introduced into the reaction chamber can also be determined.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S6,向反应室持续充入氢气,使残留的氟化氢气体排出反应室,这样可以避免残留的氟化氢气体对后续制备铝化物涂层造成影响。In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade provided by the present invention, in step S6, hydrogen is continuously charged into the reaction chamber, so that the residual hydrogen fluoride gas is discharged from the reaction chamber. Avoid the influence of residual hydrogen fluoride gas on the subsequent preparation of aluminide coatings.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S7,在持续充入氢气的状态下,气压保持预设压强,将反应室从第一预设温度以预设升温速率加热至第二预设温度,并保温第一预设时长,具体可以包括如下步骤:In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, in step S7, in the state of continuous filling of hydrogen, the air pressure is maintained at a preset pressure, and the reaction chamber is changed from The first preset temperature is heated to the second preset temperature at a preset heating rate, and the temperature is maintained for a first preset time period, which may specifically include the following steps:
S70:在持续充入氢气的状态下,气压保持15kPa~30kPa,将反应室从第一预设温度以10℃/min的升温速率加热至1000℃~1100℃,并保温1h。S70: Under the state of continuous charging of hydrogen, the air pressure is maintained at 15kPa~30kPa, and the reaction chamber is heated from the first preset temperature to 1000°C~1100°C at a heating rate of 10°C/min, and kept for 1 hour.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S8,保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持预设压强,继续保温第三预设时长;其中,预热管道的温度为第三预设温度,具体可以包括如下步骤:In specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating of complex inner cavity blades provided by the present invention, in step S8, after the heat preservation is completed, hydrogen chloride gas and hydrogen gas passing through the preheating pipeline are continuously fed into the reaction chamber and argon gas, the air pressure is maintained at the preset pressure, and the temperature is maintained for a third preset time period; wherein, the temperature of the preheating pipeline is the third preset temperature, which may specifically include the following steps:
S80:保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持15kPa~30kPa,继续保温1h~3h;其中,预热管道的温度为200℃~300℃。S80: After the heat preservation is completed, the hydrogen chloride gas, hydrogen gas and argon gas passing through the preheating pipeline are continuously introduced into the reaction chamber, the pressure is maintained at 15kPa~30kPa, and the heat preservation is continued for 1h~3h; wherein, the temperature of the preheating pipeline is 200℃~300℃ .
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S8中,向反应室通入的氯化氢气体的流量可以控制在0.5L/min~1L/min范围,氩气流量、氢气流量和氯化氢气体流量的比例可以为10:10:1,由此,向反应室通入的氢气和氩气的流量也可以确定。In the specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating of complex inner cavity blades provided by the present invention, in step S8, the flow rate of hydrogen chloride gas introduced into the reaction chamber can be controlled at 0.5L/min~ In the range of 1L/min, the ratio of argon gas flow, hydrogen gas flow and hydrogen chloride gas flow can be 10:10:1, thus, the flow rates of hydrogen and argon introduced into the reaction chamber can also be determined.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,铝化物涂层的厚度主要由步骤S8中化学气相沉积渗铝过程中保温的第三预设时长来控制,铝化物涂层的厚度可以控制在20μm~50μm范围。In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation for a complex inner cavity blade provided by the present invention, the thickness of the aluminide coating is mainly determined by the third heat preservation during the chemical vapor deposition aluminizing process in step S8. The thickness of the aluminide coating can be controlled in the range of 20 μm to 50 μm.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S4和S8中所使用的用于处理反应后尾气的碱性溶液的酸碱度优选12~13,该酸碱度的碱性溶液可以避免碱性过大对水环泵或管道造成损害,同时也能保证对于尾气中的酸性气体有良好的吸收效果。In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, the pH of the alkaline solution used in steps S4 and S8 for treating the tail gas after the reaction is preferably 12 ~13, the alkaline solution of this pH can avoid damage to the water ring pump or pipeline caused by excessive alkalinity, and can also ensure a good absorption effect on the acid gas in the tail gas.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,氢气、氩气、氟化氢气体以及氯化氢气体的纯度均为99.9%,使用纯度高的气体可以避免混入其他类型的干扰气体,从而保证涂层的制备不会受到影响。In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, the purity of hydrogen gas, argon gas, hydrogen fluoride gas and hydrogen chloride gas are all 99.9%, and the gas with high purity is used. The incorporation of other types of interfering gases can be avoided, thus ensuring that the preparation of the coating is not affected.
实施例2:Example 2:
在执行本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中的步骤S4时,向反应室持续通入的用于氟离子清洗的气体为氟利昂气体和氢气。使用氟利昂气体而非氟化氢气体的原因为:氟化氢气体在日常生产过程中有一定的危险性,用氟利昂气体代替氟化氢气体可以在提高安全性的同时仍然能达到氟离子清洗的作用。When performing step S4 in the method for fluoride ion cleaning and aluminide coating preparation of the complex inner cavity blade provided by the present invention, the gases continuously fed into the reaction chamber for fluoride ion cleaning are freon gas and hydrogen gas. The reason for using freon gas instead of hydrogen fluoride gas is: hydrogen fluoride gas has certain dangers in the daily production process. Using freon gas instead of hydrogen fluoride gas can improve safety while still achieving the effect of fluoride ion cleaning.
在具体实施时,在执行本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中的步骤S1时,可以在反应室内的石墨迷宫中放入50g~100g的铝块。具体地,铝块的投放量可以根据石墨迷宫的迷宫通道的长度来确定。In specific implementation, when performing step S1 in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, 50g-100g aluminum blocks may be placed in the graphite labyrinth in the reaction chamber. Specifically, the throwing amount of the aluminum block can be determined according to the length of the labyrinth channel of the graphite labyrinth.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S3,停止通入氩气,向反应室持续充入氢气,气压保持预设压强,将反应室从室温以预设升温速率加热至第一预设温度,并保温第一预设时长,具体可以包括如下步骤:In specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating for complex inner cavity blades provided by the present invention, in step S3, the supply of argon gas is stopped, and hydrogen gas is continuously filled into the reaction chamber, and the gas pressure is maintained at a preset pressure , heating the reaction chamber from room temperature to a first preset temperature at a preset heating rate, and maintaining the temperature for a first preset time period, which may specifically include the following steps:
S30:停止通入氩气,向反应室持续充入氢气,气压保持15kPa~30kPa,将反应室从室温以10℃/min的升温速率加热至950℃~1000℃,并保温1h。S30: Stop feeding argon gas, continue to charge hydrogen into the reaction chamber, keep the air pressure at 15kPa to 30kPa, heat the reaction chamber from room temperature to 950°C to 1000°C at a heating rate of 10°C/min, and keep the temperature for 1 hour.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S4,保温结束后,向反应室持续通入氢气和氟利昂气体,气压保持预设压强,继续保温第二预设时长,具体可以包括如下步骤:In the specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating for a complex inner cavity blade provided by the present invention, in step S4, after the heat preservation is completed, hydrogen and freon gas are continuously introduced into the reaction chamber, and the gas pressure is maintained at a preset value pressure, and continue to keep warm for a second preset time period, which may specifically include the following steps:
S40:保温结束后,向反应室持续通入氢气和氟利昂气体,气压保持15kPa~30kPa,继续保温1h。S40: After the heat preservation is completed, hydrogen and freon gas are continuously introduced into the reaction chamber, the air pressure is maintained at 15 kPa to 30 kPa, and the heat preservation is continued for 1 hour.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S4中,向反应室通入的氟利昂气体的流量可以控制在0.5L/min~1L/min范围,氢气流量与氟利昂气体流量的比例可以为10:1,由此,向反应室通入的氢气的流量也可以确定。In the specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, in step S4, the flow rate of Freon gas introduced into the reaction chamber can be controlled at 0.5L/min~ In the range of 1L/min, the ratio of the hydrogen flow rate to the freon gas flow rate can be 10:1, and thus, the flow rate of hydrogen gas introduced into the reaction chamber can also be determined.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S6,向反应室持续充入氢气,使残留的氟利昂气体排出反应室,这样可以避免残留的氟利昂气体对后续制备铝化物涂层造成影响。In the specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating for a complex inner cavity blade provided by the present invention, in step S6, hydrogen is continuously filled into the reaction chamber, so that the residual Freon gas is discharged from the reaction chamber, so that the Avoid residual Freon gas from affecting the subsequent preparation of aluminide coatings.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S7,在持续充入氢气的状态下,气压保持预设压强,将反应室从第一预设温度以预设升温速率加热至第二预设温度,并保温第一预设时长,具体可以包括如下步骤:In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, in step S7, in the state of continuous filling of hydrogen, the air pressure is maintained at a preset pressure, and the reaction chamber is changed from The first preset temperature is heated to the second preset temperature at a preset heating rate, and the temperature is maintained for a first preset time period, which may specifically include the following steps:
S70:在持续充入氢气的状态下,气压保持15kPa~30kPa,将反应室从第一预设温度以10℃/min的升温速率加热至1000℃~1100℃,并保温1h。S70: Under the state of continuous charging of hydrogen, the air pressure is maintained at 15kPa~30kPa, and the reaction chamber is heated from the first preset temperature to 1000°C~1100°C at a heating rate of 10°C/min, and kept for 1 hour.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S8,保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持预设压强,继续保温第三预设时长;其中,预热管道的温度为第三预设温度,具体可以包括如下步骤:In specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating of complex inner cavity blades provided by the present invention, in step S8, after the heat preservation is completed, hydrogen chloride gas and hydrogen gas passing through the preheating pipeline are continuously fed into the reaction chamber and argon gas, the air pressure is maintained at the preset pressure, and the temperature is maintained for a third preset time period; wherein, the temperature of the preheating pipeline is the third preset temperature, which may specifically include the following steps:
S80:保温结束后,向反应室持续通入经过预热管道的氯化氢气体、氢气和氩气,气压保持15kPa~30kPa,继续保温1h~3h;其中,预热管道的温度为200℃~300℃。S80: After the heat preservation is completed, the hydrogen chloride gas, hydrogen gas and argon gas passing through the preheating pipeline are continuously introduced into the reaction chamber, the pressure is maintained at 15kPa~30kPa, and the heat preservation is continued for 1h~3h; wherein, the temperature of the preheating pipeline is 200℃~300℃ .
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S8中,向反应室通入的氯化氢气体的流量可以控制在0.5L/min~1L/min范围,氩气流量、氢气流量和氯化氢气体流量的比例可以为10:10:1,由此,向反应室通入的氢气和氩气的流量也可以确定。In the specific implementation, in the above-mentioned method for cleaning fluoride ions and preparing aluminide coating of complex inner cavity blades provided by the present invention, in step S8, the flow rate of hydrogen chloride gas introduced into the reaction chamber can be controlled at 0.5L/min~ In the range of 1L/min, the ratio of argon gas flow, hydrogen gas flow and hydrogen chloride gas flow can be 10:10:1, thus, the flow rates of hydrogen and argon introduced into the reaction chamber can also be determined.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,铝化物涂层的厚度主要由步骤S8中化学气相沉积渗铝过程中保温的第三预设时长来控制,铝化物涂层的厚度可以控制在20μm~50μm范围。In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation for a complex inner cavity blade provided by the present invention, the thickness of the aluminide coating is mainly determined by the third heat preservation during the chemical vapor deposition aluminizing process in step S8. The thickness of the aluminide coating can be controlled in the range of 20 μm to 50 μm.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,步骤S4和S8中所使用的用于处理反应后尾气的碱性溶液的酸碱度优选12~13,该酸碱度的碱性溶液可以避免碱性过大对水环泵或管道造成损害,同时也能保证对于尾气中的酸性气体有良好的吸收效果。In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, the pH of the alkaline solution used in steps S4 and S8 for treating the tail gas after the reaction is preferably 12 ~13, the alkaline solution of this pH can avoid damage to the water ring pump or pipeline caused by excessive alkalinity, and can also ensure a good absorption effect on the acid gas in the tail gas.
在具体实施时,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中,氢气、氩气、氟利昂气体以及氯化氢气体的纯度均为99.9%,使用纯度高的气体可以避免混入其他类型的干扰气体,从而保证涂层的制备不会受到影响。In specific implementation, in the above-mentioned method for fluoride ion cleaning and aluminide coating preparation of complex inner cavity blades provided by the present invention, the purity of hydrogen gas, argon gas, freon gas and hydrogen chloride gas are all 99.9%, and high-purity gas is used. The incorporation of other types of interfering gases can be avoided, thus ensuring that the preparation of the coating is not affected.
基于同一发明构思,本发明还提供了一种复杂内腔叶片氟离子清洗及铝化物涂层制备的装置,如图3所示,包括:反应室7、石墨迷宫8、叶片工装9、渗铝通道10、氟离子清洗通道11、气体产生室12、热电偶13及金属网14;其中,Based on the same inventive concept, the present invention also provides a device for fluoride ion cleaning and aluminide coating preparation of a complex inner cavity blade, as shown in Figure 3, including: a
石墨迷宫8和叶片工装9位于反应室7内,叶片工装9用于安装叶片15,叶片15安装于叶片工装9的上方,叶片工装9位于石墨迷宫8的上方;石墨迷宫8具有迷宫通道,迷宫通道用于放置铝块,迷宫通道的出气口对准安装于叶片工装9上的叶片15的榫头16,迷宫通道的进气口与位于反应室7外的渗铝通道10连通,气体产生室12位于渗铝通道10上,气体产生室12用于放置铝块,渗铝通道10用于通入氯化氢气体、氢气和氩气,渗铝通道10内的气体经过气体产生室12后经过迷宫通道,从迷宫通道的出气口进入叶片15;The
氟离子清洗通道11在气体产生室12与迷宫通道进气口之间的位置嵌套进渗铝通道10内,从石墨迷宫8的中心穿过直至迷宫通道的出气口处;氟离子清洗通道11用于通入氟化氢气体、氢气和氩气,或者通入氟利昂气体、氢气和氩气;The fluoride
金属网14位于氟离子清洗通道11的出气口处,可以拆卸清洗,金属网14用于阻挡在高温时氟利昂气体与氢气反应生成的碳进入叶片15,从而可以避免在高温时氟利昂气体与氢气反应生成的碳在叶片15的表面沉积;The
热电偶13位于反应室7的内壁上,用于对反应室7内的温度进行测量,如图3所示,可以在反应室7内壁的上中下三个位置分别设置热电偶13,这样,可以保证整个反应室7内的温度一致;The
反应室7的底部设有用于排出反应尾气的排气口17。The bottom of the
需要说明的是,在本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的装置中,对于上述实施例1,在执行本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法中的步骤S4时,向反应室持续通入的用于氟离子清洗的气体为氟化氢气体和氢气的情况,可以省去金属网的设置,如图4所示,这是由于在高温时氟化氢气体和氢气不会反应生成碳,因此,无需设置金属网进行过滤。It should be noted that, in the device for fluoride ion cleaning and aluminide coating preparation of the complex inner cavity blade provided by the present invention, for the above embodiment 1, the above complex inner cavity blade fluoride ion cleaning and aluminum compound coating provided by the present invention are performed. In step S4 in the method for preparing the compound coating, in the case that the gases continuously fed into the reaction chamber for fluoride ion cleaning are hydrogen fluoride gas and hydrogen gas, the setting of the metal mesh can be omitted, as shown in FIG. 4 , which is Since hydrogen fluoride gas and hydrogen do not react to form carbon at high temperatures, there is no need to install a wire mesh for filtration.
本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的装置,可以实现氟离子清洗和铝化物涂层制备。下面分别结合图3和图4所示的装置分别对氟离子清洗过程和铝化物涂层制备过程的具体实施例进行详细说明。The device for fluoride ion cleaning and aluminide coating preparation of the complex inner cavity blade provided by the present invention can realize fluoride ion cleaning and aluminide coating preparation. Specific embodiments of the fluoride ion cleaning process and the aluminide coating preparation process will be described in detail below with reference to the devices shown in FIG. 3 and FIG. 4 respectively.
实施例1结合图4来阐明叶片内腔的氟离子清洗过程。首先,将去油清洗或表面喷砂后的叶片15经清洗干燥后与叶片工装9组装后放置于反应室7中,并在石墨迷宫8中放入50g~100g的铝块;然后,利用真空泵抽真空,并向渗铝通道10和氟离子清洗通道11通入氩气,反复清洗反应室7中的气氛,气体通过排气口17被真空泵抽走;在反应室7中的气氛清洗干净之后,停止向渗铝通道10和氟离子清洗通道11通入氩气,从渗铝通道10向反应室7中通入氢气,在保持预设压强15kPa~30kPa的状态下,通过电加热的方式从室温升温至第一预设温度950℃~1000℃,升温速率为10℃/min,通过上、中、下三个位置的热电偶13来监控反应室不同位置的温度,到达第一预设温度之后再保温1h,确保石墨迷宫8与叶片15的温度均到达第一预定温度;接着,在保温结束后,从氟离子清洗通道11向反应室7中持续通入高纯度的氟化氢气体,并从渗铝通道10向反应室7中持续通入氢气气体,在保持预设压强15kPa~30kPa的状态下,继续保温1h,氟化氢气体穿过石墨迷宫8的中心通道而非石墨迷宫8的迷宫通道,在此期间采用大流量的气体使得氟离子清洗气氛经叶片15榫头16进气口进入至叶片15的内部空腔,确保叶片15内腔表面的氧化物与氟离子清洗气氛充分反应,并由气膜冷却孔4流出,最终从排气口17排出,尾气通过碱性溶液池后排入大气;最后,在保温结束后,停止通入氟化氢气体,完成对叶片15内腔的氟离子清洗。Embodiment 1 illustrates the fluoride ion cleaning process of the inner cavity of the blade in conjunction with FIG. 4 . First, the
实施例2结合图3来阐明叶片内腔的氟离子清洗过程。首先,将去油清洗或表面喷砂后的叶片15经清洗干燥后与叶片工装9组装后放置于反应室7中,并在石墨迷宫8中放入50g~100g的铝块;然后,利用真空泵抽真空,并向渗铝通道10和氟离子清洗通道11通入氩气,反复清洗反应室7中的气氛,气体通过排气口17被真空泵抽走;在反应室7中的气氛清洗干净之后,停止向渗铝通道10和氟离子清洗通道11通入氩气,从渗铝通道10向反应室7中通入氢气,在保持预设压强15kPa~30kPa的状态下,通过电加热的方式从室温升温至第一预设温度950℃~1000℃,升温速率为10℃/min,通过上、中、下三个位置的热电偶13来监控反应室不同位置的温度,到达第一预设温度之后再保温1h,确保石墨迷宫8与叶片15的温度均到达第一预定温度;接着,在保温结束后,从氟离子清洗通道11向反应室7中持续通入高纯度的氟利昂气体和氢气,并从渗铝通道10向反应室7中也持续通入氢气气体,在保持预设压强15kPa~30kPa的状态下,继续保温1h,氟利昂气体穿过石墨迷宫8的中心通道而非石墨迷宫8的迷宫通道,在此期间采用大流量的气体使得氟离子清洗气氛经叶片15榫头16进气口进入至叶片15的内部空腔,确保叶片15内腔表面的氧化物与氟离子清洗气氛充分反应,并由气膜冷却孔4流出,最终从排气口17排出,尾气通过碱性溶液池后排入大气;最后,在保温结束后,停止通入氟利昂气体,完成对叶片15内腔的氟离子清洗。Embodiment 2 illustrates the fluoride ion cleaning process of the inner cavity of the blade in conjunction with FIG. 3 . First, the
结合图3和图4来阐明通过化学气相沉积法渗铝在叶片表面及内腔制备铝化物涂层的过程。首先,通过渗铝通道10和氟离子清洗通道11充入氢气,清洗反应室7内的气氛;然后,在持续充入氢气保持预设压强15kPa~30kPa的状态下,通过电加热的方式将反应室7从第一预设温度加热至第二预设温度1000℃~1100℃,升温速率为10℃/min,到达第二预设温度之后再保温1h,确保石墨迷宫8和叶片15到达第二预定温度;接着,在保温结束后,氟离子清洗通道11停止充入氢气,通过渗铝通道10向反应室7中持续通入经过温度为300℃的预热管道的氯化氢气体、氢气和氩气,在保持预设压强15kPa~30kPa的状态下,继续保温1h~3h,渗铝气氛穿过石墨迷宫8中放置铝块的迷宫通道而非石墨迷宫8的中心通道,在此期间保持水环泵持续工作,让渗铝气氛充分地流经叶片15的每个结构,经叶片15榫头16进气口进入至叶片15的内部空腔并由气膜冷却孔4流出,最终从排气口17排出,尾气通过碱性溶液池后排入大气;最后,在保温结束之后,停止通入氯化氢气体和氢气,保持从渗铝通道10通入氩气至叶片15,待叶片15随反应室7冷却至室温后,停止抽真空,待反应室7压强升至大气压后,停止通入氩气,开仓取叶片15,完成叶片15的铝化物涂层制备。渗铝通道10通入的氢气和氯化氢气体在200℃~300℃下与气体产生室12中的铝块反应生成三氯化铝气体,氩气作为载气载着三氯化铝进入石墨迷宫8,在1000℃~1100℃下三氯化铝与石墨迷宫8中的铝块和氢气进一步反应生成二氯化铝和一氯化铝,在氩气载气的推动下二氯化铝和一氯化铝到达叶片15内部空腔表面和外表面,活性较高的二氯化铝和活性高的一氯化铝与基底(即叶片15内腔表面和外表面)元素反应形成渗铝涂层。3 and 4 to illustrate the process of preparing aluminide coating on the blade surface and inner cavity by chemical vapor deposition aluminizing. First, hydrogen is charged through the aluminizing
本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法及装置,通过化学气相沉积法(CVD)对叶片内腔进行氟离子清洗和铝化物涂层制备,叶片内腔氟离子清洗的目的是去除内腔壁残留的氧化物层,为后续化学气相沉积法制备渗铝涂层提供条件。氟离子清洗和铝化物涂层制备这两个过程都是采用CVD设备完成,并且这两个过程之间无需打开CVD设备,无需取出叶片,两个过程在CVD设备中一体化完成,不仅可以节约处理时间,还可以避免因中途取出叶片而对叶片造成二次污染,上述方法灵活可控,制备的铝化物涂层的清洁度高,且不会损伤叶片。本发明提供的上述复杂内腔叶片氟离子清洗及铝化物涂层制备的方法,尤其适用于具有复杂内腔结构的镍基单晶高温合金导向器叶片及高压涡轮叶片内腔及表面高温防护涂层的化学气相沉积法制备,同时也适用于其他高温合金零部件防护涂层的制备。The method and device for fluoride ion cleaning and aluminide coating preparation of the above-mentioned complex inner cavity blade provided by the present invention, the blade inner cavity is cleaned by fluoride ion and aluminide coating is prepared by chemical vapor deposition (CVD), and the blade inner cavity fluorine The purpose of ion cleaning is to remove the residual oxide layer on the inner cavity wall and provide conditions for the subsequent preparation of aluminized coating by chemical vapor deposition. The two processes of fluoride ion cleaning and aluminide coating preparation are both completed by CVD equipment, and there is no need to open the CVD equipment or take out the blades between the two processes. The two processes are integrated in the CVD equipment, which not only saves money The processing time can also avoid secondary pollution of the leaves due to the removal of the leaves in the middle. The above method is flexible and controllable, and the prepared aluminide coating has high cleanliness and will not damage the leaves. The method for fluoride ion cleaning and aluminide coating preparation of the above-mentioned complex inner cavity blade provided by the present invention is especially suitable for nickel-based single crystal superalloy guide blades with complex inner cavity structure and high-pressure turbine blade inner cavity and surface high temperature protective coating It is also suitable for the preparation of protective coatings for other superalloy parts.
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention. Thus, provided that these 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 these modifications and variations.
Claims (6)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011071362.1A CN112430802B (en) | 2020-10-09 | 2020-10-09 | Method and device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011071362.1A CN112430802B (en) | 2020-10-09 | 2020-10-09 | Method and device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112430802A CN112430802A (en) | 2021-03-02 |
| CN112430802B true CN112430802B (en) | 2022-02-08 |
Family
ID=74690415
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011071362.1A Active CN112430802B (en) | 2020-10-09 | 2020-10-09 | Method and device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112430802B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150288B (en) * | 2021-11-11 | 2023-05-16 | 武汉材料保护研究所有限公司 | Seepage agent generator, chemical vapor deposition reaction device and vapor deposition method |
| CN115491634A (en) * | 2022-09-20 | 2022-12-20 | 国营川西机器厂 | Apparatus for preparing aluminized layer of aeroengine blade inner cavity |
| CN115786759B (en) * | 2022-11-11 | 2024-06-04 | 广州众山精密科技有限公司 | Equipment and method for preparing near-net-shaped aluminum-based silicon carbide foil by gas phase aluminizing |
| CN117512503A (en) * | 2023-11-02 | 2024-02-06 | 中国航发沈阳黎明航空发动机有限责任公司 | A method for preparing an aluminide infiltration layer containing silicon on the surface |
| CN117187738A (en) * | 2023-11-07 | 2023-12-08 | 中国航发沈阳黎明航空发动机有限责任公司 | Process method for vapor deposition of chromium-aluminum diffusion layer on inner and outer surfaces of hollow blade |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6224941B1 (en) * | 1998-12-22 | 2001-05-01 | General Electric Company | Pulsed-vapor phase aluminide process for high temperature oxidation-resistant coating applications |
| CN102978565A (en) * | 2012-11-20 | 2013-03-20 | 西安航空动力股份有限公司 | Seepage prevention method and fixture for aerial engine blade rabbet |
| CN103993258A (en) * | 2014-05-21 | 2014-08-20 | 昆山海普电子材料有限公司 | Method for coating workpiece with complex inner cavity structure |
| CN105695929A (en) * | 2016-02-29 | 2016-06-22 | 北京航空航天大学 | Method for preparing protective coating suitable for blade with high Mo content and complex inner cavity structure |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10224632A1 (en) * | 2002-06-04 | 2003-12-24 | Mtu Aero Engines Gmbh | Process for the internal coating of gas turbine blades |
| US7026011B2 (en) * | 2003-02-04 | 2006-04-11 | General Electric Company | Aluminide coating of gas turbine engine blade |
| US10533255B2 (en) * | 2015-08-27 | 2020-01-14 | Praxair S.T. Technology, Inc. | Slurry formulations for formation of reactive element-doped aluminide coatings and methods of forming the same |
-
2020
- 2020-10-09 CN CN202011071362.1A patent/CN112430802B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6224941B1 (en) * | 1998-12-22 | 2001-05-01 | General Electric Company | Pulsed-vapor phase aluminide process for high temperature oxidation-resistant coating applications |
| CN102978565A (en) * | 2012-11-20 | 2013-03-20 | 西安航空动力股份有限公司 | Seepage prevention method and fixture for aerial engine blade rabbet |
| CN103993258A (en) * | 2014-05-21 | 2014-08-20 | 昆山海普电子材料有限公司 | Method for coating workpiece with complex inner cavity structure |
| CN105695929A (en) * | 2016-02-29 | 2016-06-22 | 北京航空航天大学 | Method for preparing protective coating suitable for blade with high Mo content and complex inner cavity structure |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112430802A (en) | 2021-03-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112430802B (en) | Method and device for cleaning fluorine ions of blades with complex inner cavities and preparing aluminide coatings | |
| JP5965132B2 (en) | Turbine component with cooling features and method of manufacturing the same | |
| EP1790753B1 (en) | Duplex gas phase coating | |
| EP2253464B1 (en) | Graded platinum diffusion aluminide coating | |
| US9238265B2 (en) | Backstrike protection during machining of cooling features | |
| EP1795629A2 (en) | Oxide cleaning and coating of metallic components | |
| JP5483854B2 (en) | Method for aluminum coating of turbomachinery hollow metal parts in the gas phase | |
| CN105296956B (en) | A kind of cobalt-base alloys blade inner chamber and the process of outer surface aluminising | |
| CN105695929B (en) | A kind of preparation method suitable for high Mo content complicated inner cavity structure blade protective coating | |
| JP2022551859A (en) | Method for depositing a protective anti-coking coating on an aerospace component | |
| EP3066227B1 (en) | Method for producing diffusion aluminide coatings | |
| EP1895019B1 (en) | Method and apparatus for controlling diffusion coating of internal passages | |
| EP2947174B1 (en) | Method for slurry aluminide coating repair | |
| CN107675120B (en) | A method for preparing molybdenum silicide coating on the surface of molybdenum or molybdenum alloy | |
| WO2021045841A1 (en) | Methods for forming protective coatings containing crystallized aluminum oxide | |
| CN103434209B (en) | A kind of novel lower thermal conductivity and high temperature heat-resistant barrier coating and preparation method thereof | |
| JP2017121663A (en) | Method and assembly for forming components having internal passages using jacketed core | |
| CN116200726A (en) | A method of chemical vapor deposition AlCr coating on the surface of nickel-based superalloy | |
| JP3651710B2 (en) | Chemical vapor deposition aluminized film forming method for gas turbine blade | |
| CN112302830A (en) | A rhenium iridium-carbon carbon engine thrust chamber and its integrated preparation method | |
| US11022039B2 (en) | Method of manufacturing conductive film holes | |
| US20210381386A1 (en) | Oxide layer compositions for turbine engine components | |
| JP2610914B2 (en) | Method and apparatus for coating aluminum inside heat resistant member | |
| US20210292882A1 (en) | Coating for refractory alloy part | |
| CN112941486B (en) | A kind of molybdenum-based thermal oxidation anti-corrosion ceramic coating and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |