阅读说明：本技术 一种含有储铝层的抗氧化涂层及其制备方法 (Oxidation-resistant coating containing aluminum storage layer and preparation method thereof ) 是由 王玉锋 杨岩 张华� 雷丹 王瑞 杨鹏 王丽 张盟 于 2020-06-30 设计创作，主要内容包括：本发明公开了一种含有储铝层的抗氧化涂层及其制备方法,该制备方法通过在渗透的过程,将渗铝剂FeAl粉和催化剂加入至渗罐中,通过渗透处理,在叶片基体的表面形成一层储铝层。渗透过程中采用普通马弗罐进行气相渗Al,工艺简单,操作简便,设备要求低,装炉量大,通过对比发现在相同的热防护涂层厚度条件下,气相渗Al生产成本较电弧离子镀生产成本降低98.2％。(The invention discloses an anti-oxidation coating containing an aluminum storage layer and a preparation method thereof. The common muffle tank is adopted for carrying out gas phase Al infiltration in the infiltration process, the process is simple, the operation is simple and convenient, the equipment requirement is low, the furnace loading amount is large, and the comparison shows that the production cost of the gas phase Al infiltration is reduced by 98.2 percent compared with the production cost of the electric arc ion plating under the condition of the same thickness of the thermal protection coating.)

1. A preparation method of an oxidation resistant coating containing an aluminum storage layer is characterized by comprising the following steps:

step 1, cleaning the surface of a blade substrate through pretreatment;

step 2, baking FeAl powder;

step 3, preparing an aluminum storage layer;

the roasted FeAl powder and a catalyst NH₄I, placing the pretreated blade substrate into an infiltration tank, replacing the atmosphere in the infiltration tank with argon gas by using 6-10 Kg of FeAl powder infiltration agent for every 40-60 blade substrates, heating the infiltration tank to 950-1000 ℃, preserving heat for 8-15H, and preparing an aluminum storage layer on the surface of the blade substrate;

carrying out vacuum heat treatment on the blade substrate attached with the aluminum storage layer at 1000-1050 ℃ for 2-15H to obtain the blade substrate attached with the aluminum storage layer after heat treatment;

step 4, preparing the MCrAlY coating;

preparing an MCrAlY coating on the surface of the blade substrate attached with the aluminum storage layer through arc ion plating;

step 5, diffusion treatment;

placing the blade substrate attached with the aluminum storage layer and the MCrAlY coating prepared in the step (4) into a furnace for heat treatment;

the oxidation-resistant coating containing the aluminum storage layer is prepared through the steps.

2. The method for preparing the oxidation-resistant coating containing the aluminum storage layer as claimed in claim 1, wherein the pretreatment in step 1 comprises dry sand blowing, argon blow drying, ultrasonic cleaning and drying in sequence.

3. The method for preparing an oxidation resistant coating containing an aluminum storage layer as claimed in claim 1, wherein in step 2, NH is used for every 40-60 blade substrates₄I 300～500g。

4. The method for preparing the oxidation-resistant coating containing the aluminum storage layer as claimed in claim 1, wherein in the step 2, the baking temperature is 100-200 ℃ and the baking time is 1-10H.

5. The method for preparing an oxidation resistant coating containing an aluminum storage layer as claimed in claim 1, wherein in the step 3, the argon gas replacement process comprises: pumping the vacuum degree in the infiltration tank to be less than or equal to 1Pa, then introducing argon to the pressure in the tank to be 0.1-1 MPa, repeating the steps for at least 5 times, pumping the vacuum in the infiltration tank to be less than 1Pa in the last time, and introducing argon to be 0.05-1 MPa.

6. The method for preparing the anti-oxidation coating containing the aluminum storage layer as claimed in claim 1, wherein in the step 3, the pressure in the infiltration tank is 0.05-1 MPa in the heat preservation process.

7. The method for preparing the oxidation resistant coating containing the aluminum storage layer as claimed in claim 1, wherein in the step 4, the MCrAlY coating is prepared under a vacuum pressure of 0.3 +/-0.15 Pa and a coating time of 5-10 h.

8. The method for preparing the oxidation-resistant coating containing the aluminum storage layer as claimed in claim 1, wherein the diffusion treatment of step 5 is performed after the blade substrate prepared in step 4 is cooled, and the degree of vacuum of the diffusion is less than 5 × 10^-2Pa, the diffusion temperature is 1000-1050 ℃, and the diffusion time is 1-5H.

9. An oxidation-resistant coating containing an aluminum storage layer, which is prepared by the preparation method of any one of claims 1 to 8, is characterized in that the oxidation-resistant coating comprises the aluminum storage layer and an MCrAlY coating from inside to outside in sequence, and the aluminum storage layer is attached to a blade substrate.

10. The oxidation resistant coating comprising an aluminum storage layer as claimed in claim 9, wherein the aluminum storage layer comprises 25-30% Al by weight and has a thickness of 10-50 μm.

[ technical field ] A method for producing a semiconductor device

The invention belongs to the field of high-temperature oxidation resistant coatings for turbine blades of aeroengines, and particularly relates to an oxidation resistant coating containing an aluminum storage layer and a preparation method thereof.

[ background of the invention ]

At present, the MCrAlY coating prepared by the arc ion plating technology has the advantages of compact coating structure and the like, and is widely applied to the preparation and processing of various high-temperature protective coatings of turbine blades, so that the high-temperature oxidation resistance, the corrosion resistance and the heat insulation performance of the turbine blades are obviously improved, and the service life of an engine is prolonged.

The gas-phase Al-permeating technology is that non-contact diffusion metal permeating technology is adopted, powdered permeating agent, dispersant and catalyst are mixed homogeneously, and the mixture is maintained at certain temperature for certain time to produce decomposition and reduction reaction in the hearth and form one Al-permeating layer with high temperature oxidation resistance on the surface of the workpiece.

However, when the MCrAlY coating is deposited by arc ion plating, the Al content in the coating is generally maintained at about 10% due to the process characteristics, and the concentration of the Al content cannot be further increased, which causes inward and outward diffusion of Al atoms in the service process of the coating, resulting in shortened oxidation resistance life of the coating. Therefore, on the premise of ensuring the MCrAlY coating structure, more Al atoms are urgently needed to be supplied, so that the service life of the oxidation-resistant coating is obviously prolonged.

[ summary of the invention ]

The invention aims to overcome the defects of the prior art and provides an anti-oxidation coating containing an aluminum storage layer and a preparation method thereof.

In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:

a preparation method of an oxidation resistant coating containing an aluminum storage layer comprises the following steps:

step 1, cleaning the surface of a blade substrate through pretreatment;

step 2, baking FeAl powder;

step 3, preparing an aluminum storage layer;

the roasted FeAl powder and a catalyst NH₄I, placing the pretreated blade substrate into an infiltration tank, replacing the atmosphere in the infiltration tank with argon gas by using 6-10 Kg of FeAl powder infiltration agent for every 40-60 blade substrates, heating the infiltration tank to 950-1000 ℃, preserving heat for 8-15H, and preparing an aluminum storage layer on the surface of the blade substrate;

carrying out vacuum heat treatment on the blade substrate attached with the aluminum storage layer at 1000-1050 ℃ for 2-15H to obtain the blade substrate attached with the aluminum storage layer after heat treatment;

step 4, preparing the MCrAlY coating;

preparing an MCrAlY coating on the surface of the blade substrate attached with the aluminum storage layer through arc ion plating;

step 5, diffusion treatment;

placing the blade substrate attached with the aluminum storage layer and the MCrAlY coating prepared in the step (4) into a furnace for heat treatment;

the oxidation-resistant coating containing the aluminum storage layer is prepared through the steps.

The invention is further improved in that:

preferably, in step 1, the pretreatment includes dry sand blowing, argon blowing, ultrasonic cleaning and drying, which are performed in sequence.

Preferably, in the step 2, NH is used for every 40-60 blade matrixes₄I 300～500g。

Preferably, in the step 2, the baking temperature is 100-200 ℃, and the baking time is 1-10H.

Preferably, in step 3, the process of replacing argon is as follows: pumping the vacuum degree in the infiltration tank to be less than or equal to 1Pa, then introducing argon to the pressure in the tank to be 0.1-1 MPa, repeating the steps for at least 5 times, pumping the vacuum in the infiltration tank to be less than 1Pa in the last time, and introducing argon to be 0.05-1 MPa.

Preferably, in the step 3, the pressure in the infiltration tank is 0.05-1 MPa in the heat preservation process.

Preferably, in the step 4, when the MCrAlY coating is prepared, the vacuum pressure is 0.3 +/-0.15 Pa, and the coating time is 5-10 h.

Preferably, after cooling the blade matrix obtained in the step 4, the diffusion treatment of the step 5 is carried out, and the diffusion vacuum degree is less than 5 × 10^-2Pa, the diffusion temperature is 1000-1050 ℃, and the diffusion time is 1-5H.

The oxidation-resistant coating containing the aluminum storage layer prepared by any one of the preparation methods sequentially comprises the aluminum storage layer and the MCrAlY coating from inside to outside, and the aluminum storage layer is attached to the blade substrate.

Preferably, the mass percent of Al in the aluminum storage layer is 25-30%, and the thickness of the aluminum storage layer is 10-50 μm.

Compared with the prior art, the invention has the following beneficial effects:

the invention discloses a preparation method of an oxidation-resistant coating containing an aluminum storage layer, which comprises the steps of adding an aluminizing agent FeAl powder and a catalyst into an infiltration tank in the infiltration process, forming an aluminum storage layer on the surface of a blade substrate through infiltration treatment, and gradually diffusing the aluminum content in an attached aluminum storage layer into the blade substrate through heat treatment after the aluminizing treatment is carried out on the surface of the blade substrate under the catalysis of ammonium iodide in the infiltration process, so that the bonding force between the attached aluminum storage layer and the blade substrate is firmer. Adopt ordinary muffle tank to carry out the gas phase to ooze Al in the infiltration process, simple process, easy and simple to handle, equipment requirement is low, and the charge volume is big, discovers through the contrast that under the same hot protective coating thickness condition, the gas phase oozes Al manufacturing cost and electric arc ion plating manufacturing cost reduces 98.2%, and equipment depreciation is equivalent with when oozing Al with fuel power cost, and every electric arc ion plating target is 2980 yuan, 14 targets in every stove, 36 blade base members of coprocessing, every expense on average: 1158 element. At the same time, each kilogram of FeAl powder is 103 yuan, each 100g of NH₄50 yuan I powder, each furnace can process 36 bladesThe matrix needs 6Kg of FeAl powder and NH₄300g of I powder, the cost for processing each blade substrate is only 21 yuan on average, and the method can be seen to save 1137 yuan on average and about 98.2% of cost for aluminizing on the blade substrate relative to the arc ion plating target material.

Furthermore, through a plurality of processes of pretreatment, the blade base body can be sufficiently cleaned before use, and the subsequent aluminizing process is ensured not to have impurities between the blade base body and the aluminum storage layer.

Furthermore, the quantity of the blade substrate, the dosage of the aluminizing agent and the catalyst are limited, the blade substrate can be fully permeated, and the cost is controllable.

Further, baking is carried out before the aluminizing agent FeAl powder is used, so that the aluminizing agent does not contain moisture in the using process.

Furthermore, preparation is made for subsequent permeation through multiple times of argon replacement, so that the whole permeation process is protected by inert gas, Al is prevented from being oxidized, the aluminum content of the aluminum storage layer is prevented from being influenced, and meanwhile, the blade substrate can be prevented from being oxidized.

Furthermore, the pressure in the infiltration tank is limited, and the infiltration process is ensured to be in the protective atmosphere.

Further, after the MCrAlY coating is prepared, heat treatment is carried out, and the atomic bonding force between the aluminum storage layer and the MCrAlY coating is enhanced.

The invention also discloses an anti-oxidation coating containing the aluminum storage layer, which comprises the aluminum storage layer and the MCrAlY coating from inside to outside in sequence, wherein the aluminum storage layer is additionally arranged between the MCrAlY coating and the blade substrate and is used for supporting the MCrAlY coating in the service process, the prepared anti-oxidation coating has higher Al content and can prolong the service life of the coating, so that the substrate material has longer service life, the coating is suitable for various blades, and the blade can be provided with the MCrAlY coating on the surface.

[ description of the drawings ]

FIG. 1 is the microstructure of the anti-oxidation coating containing Al storage layer in example 1;

FIG. 2 is a graph showing the change in the Al element composition of the anti-oxidation coating layer containing Al storage layer in example 1;

FIG. 3 is the microstructure of the anti-oxidation coating containing Al storage layer in example 2;

FIG. 4 is a graph showing the change in the Al element composition of the anti-oxidation coating layer containing Al storage layer in example 2;

FIG. 5 is the microstructure of the anti-oxidation coating containing Al storage layer in example 3;

FIG. 6 is a graph showing the change of Al element composition of the anti-oxidation coating layer containing Al storage layer in example 3.

[ detailed description ] embodiments

The invention is described in further detail below with reference to the accompanying drawings:

in the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly and encompass, for example, both fixed and removable connections; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

The invention discloses an Al storage layer-containing anti-oxidation coating and a preparation method thereof.

The specific processing steps of the thermal barrier coating are as follows:

(1) and (4) pretreatment.

Before preparing the Al-infiltrated bonding layer, the blade matrix is pretreated, and the pretreatment process sequentially comprises the following steps: dry blowing sand, argon blowing, ultrasonic cleaning and drying.

(2) Baking alumetizing agent

Baking the aluminizing agent FeAl powder for 1-10H at the temperature of 100-200 ℃.

(3) And preparing a vapor phase Al-infiltrated bonding layer.

Loading the pretreated blades and the roasted penetrant into a special tool, putting the tool and the blade matrix into a penetration tank together, closing a furnace door, and using 6-10 Kg of FeAl powder penetrant and NH for every 40-60 blade matrixes₄300-500 g of I catalyst; vacuumizing to less than or equal to 1Pa by using a mechanical pump and a Roots pump, then introducing argon to 0.1-1 MPa, performing replacement treatment on air in the furnace for not less than 5 times by using the argon, and finally introducing the argon to 0.05-1 MPa. Heating to 950-1000 ℃, and preserving heat for 8-15H, wherein in the heat preservation process, when the pressure is more than 2MPa, the gas is discharged to 0.05-1 MPa. And after the heat preservation time in the furnace is finished, carrying out vacuum heat treatment for 2-15H at the temperature of 1000-1050 ℃.

(4) And preparing the MCrAlY coating by arc ion plating.

The method specifically comprises the following steps:

vacuumizing, namely vacuumizing the furnace to ensure that the pressure is lower than 5 × 10^-3Pa。

Setting a rotating speed: the rotation speed is set to 1 to 5 rpm/min.

And (3) heating: the temperature is set to 300 to 400 ℃.

Gas ion cleaning: and filling argon into the furnace chamber to ensure that the vacuum pressure reaches 0.2-0.5 Pa. Pulse bias voltage: 200 +/-50V; duty ratio: 80 plus or minus 20 percent; arc flow: 50 +/-10A; the time is 20 +/-10 min.

Film coating: argon is filled into the heating chamber, and the vacuum pressure reaches 0.3 +/-0.15 Pa. DC bias voltage: 100 +/-20V; arc source current: 100 +/-10A; coating time: 5-10 h.

Cooling and discharging: firstly, after the film coating is finished, an arc power supply is turned off, a gas source is turned off, and the workpiece rotating frame is stopped; cooling the workpiece to below 100 ℃ in a vacuum chamber, filling air into the vacuum chamber, opening a furnace door after the workpiece is balanced with the external pressure, wearing clean cotton gloves to take out the blade base body and the test piece; thirdly, wrapping the discharged blade matrix and the test piece with clean industrial soft paper.

(5) And (5) diffusion treatment.

The workpiece which is obtained in the step (4) and is taken out of the furnace is processed in a vacuum degree of less than 5 × 10^-2And (4) carrying out diffusion treatment under the conditions of Pa, temperature of 1000-1050 ℃ and heat preservation for 1-5H.

Through the above 5 steps, the anti-oxidation coating containing the aluminum storage layer is prepared, and the anti-oxidation coating containing the aluminum storage layer sequentially comprises the aluminum storage layer and the MCrAlY coating from bottom to top, wherein the aluminum storage layer is attached to the blade substrate. The aluminum content in the aluminum storage layer is 25% -30%, the thickness of the aluminum storage layer is 10-50 μm, and the components in the aluminum storage layer contain other elements of the blade matrix besides aluminum, because the elements in the blade matrix are brought into the aluminum storage layer in the infiltration and subsequent heat treatment processes.