CN114507075B - Preparation method of self-healing powder with double-shell structure - Google Patents

Preparation method of self-healing powder with double-shell structure Download PDF

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CN114507075B
CN114507075B CN202210261213.4A CN202210261213A CN114507075B CN 114507075 B CN114507075 B CN 114507075B CN 202210261213 A CN202210261213 A CN 202210261213A CN 114507075 B CN114507075 B CN 114507075B
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CN114507075A (en
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崔世宇
易周
黄�俊
罗军明
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Nanchang Hangkong University
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Abstract

The preparation method of the self-healing powder with the double-shell structure prepares the core MoSi through twice liquid phase precipitation and sintering 2 The inner shell is Al 2 O 3 The outer shell is Y 2 O 3 In the form of MoSi 2 @Al 2 O 3 @Y 2 O 3 Self-healing powder. The preparation method is simple and convenient, the components and the thickness of the shell layer are controllable, and one-time sintering of Al is avoided 2 O 3 The change in volume of the phase change causes voids and coating of Al (OH) 3 The hard agglomeration of the powder after the shell is dried is generated, and MoSi is improved 2 Compared with the sol-gel method, the cost of the antioxidant performance of the method is greatly reduced. The self-healing powder of the invention is evenly and completely coated and Al 2 O 3 Shell and Y 2 O 3 The shell has clear interface and good combination; outer casing Y 2 O 3 The ceramic can reduce the fluidity of CMAS to improve corrosion resistance, and the inner shell Al 2 O 3 The layer has low oxygen permeability to delay MoSi 2 And (4) pre-oxidation process.

Description

Preparation method of self-healing powder with double-shell structure
Technical Field
The invention relates to a preparation method of self-healing powder with a double-shell structure, and particularly belongs to the technical field of thermal barrier coating materials.
Background
At present, the design inlet temperature of aero-engines (such as WS15, M88-2 and F135) with the thrust-weight ratio of about 10 is 1450 to 1750 ℃, and the design inlet temperature of aero-engines with the thrust-weight ratio of 15 to 20 is over 2100 ℃. Turbine blades, which are one of the main components of core machines, require the selection of alloy materials with excellent mechanical and thermophysical properties. However, the extreme service temperature of the extreme ultra-high temperature alloy (less than or equal to 1150 ℃) in the severe environment is that the preparation of a ceramic layer with low Thermal conductivity represented by a Thermal Barrier Coating (TBC) becomes a main means for prolonging the service life of the turbine blade aiming at the continuously improved service temperature. TBCs currently available for commercial use are all ceramic layer/metal bond coat constructions. Wherein NiCoCrAlY is used as a representativeThe bonding layer is deposited on the surface of the high-temperature alloy to improve the difference of the thermal expansion coefficients between the ceramic layer and the substrate and enhance the oxidation resistance of the substrate. With ZrO 2 -Y 2 O 3 (YSZ, yttria Stabilized Zirconia) is the primary representative top ceramic layer, serving as a key "thermal barrier" due to its low thermal conductivity and high chemical stability. However, TBC's life is not stable during service and its dispersion mainly results from the microstructure and the dynamics of the TBC degradation process.
Among the numerous thermal barrier coating failure behaviors, TBC failure caused by changes in service environment is referred to as a conditionally guided failure, with CaO-MgO-Al in the inner duct originating from dust, sand sources, and pozzolans 2 O 3 -SiO 2 (CMAS) particles have both impact behavior and hot corrosion properties, and are one of the most prominent forms of condition-oriented failure. In addition, the porous skeleton (porosity 3% -8%) of YSZ provides an intrusion channel for corrosive media, so that c/m-ZrO can be obtained 2 Phase transformation occurs with 3% -5% volume expansion, thereby reducing the overall strain tolerance of the coating. During the initial stages of corrosion, the YSZ ceramic layer forms an interaction zone with the glassy CMAS, where Ca 2+ The erosion damage to the coating is most pronounced because CaO and Y 2 O 3 Is an oxide of alkaline earth and rare earth metals with a doping ionic radius lower than quadrivalence, and the stabilization mechanism is that oxygen vacancies with high concentration are formed in the oxide. At the same time, caO may be present with ZrO 2 Generate chemical reaction to generate CaZrO 3 And Ca abundantly present in the interaction zone 2+ And Mg 2+ Can be dissolved into a YSZ unit cell structure in a solid solution mode to replace Y 3+ Leading to the formation of Y-poor regions in YSZ, thereby causing c/t-ZrO 2 Destabilization and phase transition. The addition of self-healing components to ceramic coatings has become another effective means of retarding coating failure in order to inhibit the formation of primary cracks.
By using MoSi 2 The concept of powder preparation of self-healing coatings arises. Dalton type metal compound MoSi 2 Combines the characteristics of ceramics and metals, has excellent high-temperature oxidation resistance, and uses MoSi 2 Made of a rodThe heating element of (a) may be heated to 1700 ℃; it has moderate density (6.24 g/cm) 3 ) The ductile-brittle transition temperature of which is up to 1000 ℃, below which MoSi is present 2 Which manifests itself as hard brittleness of the ceramic, and ductile behaviour of the metal above that temperature. And the complex parts can be obtained by using electric spark machining, so that the defect of difficult ceramic machining is overcome. Therefore, the method has strong application potential in a high-temperature environment of more than 1000 ℃. MoSi 2 Oxidized at high temperature to generate amorphous SiO with strong fluidity 2 Will bring about 138% volume expansion while SiO 2 Can flow along the microcracks and solidify to fill the microcracks when the temperature is reduced. Furthermore, siO 2 Can also be mixed with ZrO at high temperature 2 Formation of ZrSiO 4 The strength of the coating is restored. Albeit MoSi 2 The method has wide application prospect in the aspect of thermal barrier coating repair, but the problem of pre-oxidation still needs to be solved for practical application. Bulk MoSi 2 Can have excellent high-temperature oxidation resistance and benefit from MoSi 2 When oxidized, a glassy SiO forms on the surface 2 A protective layer capable of blocking the penetration of oxygen to thereby improve MoSi 2 Oxidation resistance of (2). But MoSi for thermal spraying 2 The powder has too small particle size and is difficult to form continuous and dense SiO 2 Layer of SiO 2 The layer needs to have a certain thickness to effectively block the penetration of oxygen. Therefore, coating a protective layer having low oxygen permeability on the outside is one of the options for improving the pre-oxidation resistance.
The mechanism of the core-shell powder for crack healing in thermal barrier coatings is that MoSi is located in the core when the shell is intact due to its protective effect 2 No or little oxidation. But when the coating is damaged due to the expansion of the microcracks, the cracks penetrate through the core-shell structure MoSi 2 Oxygen along crack propagation direction with MoSi in powder form 2 Contact and react. SiO produced by oxidation and having strong fluidity 2 The volume expansion flows along the crack to fill the crack, and SiO 2 Reacting with ZrO2 to form ZrSiO 4 The adhesive has an effect of repairing cracks. To enhance the resistance of YSZ materials to CMAS attack, preparationMoSi 2 @Al 2 O 3 @Y 2 O 3 Double-layer core-shell structure powder. In a CMAS corrosive environment, Y 2 O 3 Ca reacting with corrosive medium to generate oxygen-silicon apatite structure 2 Y 8 (SiO 4 ) 6 O 2 The fluidity of CMAS is reduced, and the addition of Y element is helpful to compensate Y in YSZ 2 O 3 Dynamic loss prevention of c/m-ZrO 2 A phase change occurs.
The self-healing powder prepared at present is of a single-layer shell structure and cannot effectively resist corrosion cracks caused by CMAS, and the shell layer prepared at present is prepared by sol-gel, so that the thickness of the shell layer prepared by the method is difficult to break through 100 nm, which is caused by the low solubility of organic alkoxide. Finally, the sizes of the MoSi2 powder with the core-shell structure prepared at present are all 3 to 5 mu m, and the requirement of thermal spraying powder on the flowability is not met.
Disclosure of Invention
Aiming at the situation, the invention provides a preparation method of self-healing powder with a double-shell structure, which overcomes the generation of crack propagation phenomenon in the CMAS corrosion process to prevent the failure of a coating.
The invention relates to a preparation method of self-healing powder with a double-shell structure, which uses MoSi 2 As a core material of the self-healing powder, al (NO) 3 ) 3 •9H 2 O is an aluminum source, Y (NO) 3 ) 3 •6H 2 O is yttrium source, and Al is prepared as inner shell layer by two liquid phase precipitation and sintering 2 O 3 The outer shell layer is Y 2 O 3 Of MoSi 2 @Al 2 O 3 @Y 2 O 3 The self-healing powder comprises the following specific processes:
step 1: moSi 2 @Al 2 O 3 Preparation of the powder
At the temperature of 55 ℃, 1.5 to 2.5mol/L of Al (NO) is added under the condition of stirring 3 ) 3 The solution is dropwise added with MoSi of 50g/L 2 In the suspension, ammonia water is simultaneously dripped to control the pH value of the reaction system to be 8.5-9.5; after the dropwise addition is finished, continuously stirring and preserving the heat for 1-2 hours;
carrying out solid-liquid separation on the reaction product, washing the obtained filter cake with deionized water for three times, placing the filter cake into absolute ethyl alcohol, stirring for 30min, carrying out solid-liquid separation, drying at 120 ℃ for 20h, grinding for 10 min, and sieving up and down by 150 meshes and 500 meshes to obtain MoSi 2 @Al(OH) 3 The powder is sintered for 3 to 7 hours in vacuum at 1200 ℃ and the vacuum degree of less than 10Pa, and then is sieved up and down by 150 meshes and 500 meshes to obtain MoSi 2 @Al 2 O 3 Powder;
step 2: moSi 2 @Al 2 O 3 @Y 2 O 3 Preparation of self-healing powder
At the temperature of 90 ℃, under the stirring condition, 1.5 to 2.5mol/L of Y (NO) 3 ) 3 The solution is dripped into 50g/L MoSi 2 @Al 2 O 3 The powder suspension is simultaneously dripped with ammonia water to control the pH value of a reaction system to be 6-7; after the dropwise addition is finished, continuously stirring for 1 h;
carrying out solid-liquid separation on the reaction product, drying the obtained filter cake at 120 ℃ for 20h, and grinding for 10 min to obtain MoSi 2 @Al 2 O 3 @Y(OH) 3 The powder is sintered for 3 to 7 hours in vacuum at 900 ℃, and then is sieved up and down by 150 meshes and 500 meshes to prepare the MoSi with the double-shell structure 2 @Al 2 O 3 @Y 2 O 3 Self-healing powder.
The MoSi 2 Has an average particle diameter of 30 to 50 μm.
The MoSi 2 、Al(NO 3 ) 3 •9H 2 O、Y(NO 3 ) 3 •6H 2 The mass ratio of the dosage of the three raw materials of O is 1: 8-10.
The invention has the beneficial effects that: the invention uses MoSi 2 As a core material of the self-healing powder, al (NO) 3 ) 3 •9H 2 O is an aluminum source, Y (NO) 3 ) 3 •6H 2 O is yttrium source, and Al is prepared as inner shell layer by two liquid phase precipitation and sintering 2 O 3 The outer shell layer is Y 2 O 3 Of MoSi 2 @Al 2 O 3 @Y 2 O 3 Self-healing powder. The method adopts liquid phase precipitation and sintering modes, has simple and convenient operation and controllable shell components, can obtain shells with different thicknesses according to the adjustment of technological parameters, and avoids one-time sintering of Al 2 O 3 The change in volume of the phase change causes voids and coating of Al (OH) 3 The hard agglomeration of the powder after the shell is dried is generated, and MoSi is improved 2 Compared with a sol-gel method, the cost of the antioxidant performance of the composite material is greatly reduced.
Drawings
FIG. 1 shows the preparation of MoSi according to the invention 2 @Al 2 O 3 @Y 2 O 3 A process flow diagram of self-healing powder;
FIG. 2 shows MoSi according to the present invention 2 @Al 2 O 3 A powder morphology map;
FIG. 3 shows MoSi according to the present invention 2 @Al 2 O 3 @Y 2 O 3 A powder morphology graph;
FIG. 4 shows MoSi according to the present invention 2 @Al 2 O 3 @Y 2 O 3 The cross-sectional shape of the powder;
wherein: the arrow is the EDS line scan direction;
FIG. 5 is a schematic view of: moSi of the invention 2 @Al 2 O 3 @Y 2 O 3 Scanning the EDS line of the powder section;
FIG. 6 shows MoSi according to the present invention 2 @Al 2 O 3 @Y 2 O 3 Powder oxidation weight loss curve.
Detailed Description
Example 1
80g of Al (NO) was added to 100ml of deionized water 3 ) 3 •9H 2 Preparing aluminum nitrate solution from O, and mixing 10g of MoSi with average particle size of 30-50 μm 2 Dispersing in 200ml deionized water to prepare MoSi 2 And (3) suspension. Mixing MoSi 2 The suspension was placed in a thermostatically magnetically stirred water bath at a stirring speed of 800rpm and a temperature of 55 ℃. The aluminum nitrate solution is put into a separating funnel, and the speed is controlled to slowly drop the aluminum nitrate solution into MoSi 2 Suspending liquid, and simultaneously sucking ammonia water by using a needle tube and dripping MoSi 2 Suspension controlThe pH was adjusted to 8.5. After the aluminum nitrate solution is completely dripped, continuously stirring for 1h at constant temperature, carrying out solid-liquid separation, then washing with deionized water, carrying out solid-liquid separation again, putting the solid into 400ml of absolute ethyl alcohol, stirring for 30min, carrying out solid-liquid separation, washing with absolute ethyl alcohol, and carrying out solid-liquid separation again. Drying the obtained solid in a drying box at 120 ℃ for 20h, and lightly grinding to obtain MoSi 2 @Al(OH) 3 Powder, which is put into a vacuum tube furnace to be treated for 5 hours at 1200 ℃ and kept in a vacuum state (<10 Pa) is added. Taking out and sieving to obtain MoSi 2 @Al 2 O 3 The powder has 150-mesh and 500-mesh upper and lower meshes.
80g of Y (NO) was added to 100ml of deionized water 3 ) 3 •6H 2 O into yttrium nitrate solution, 10g of MoSi 2 @Al 2 O 3 The powder is dispersed in 200ml deionized water to prepare MoSi 2 @Al 2 O 3 And (3) suspension. Mixing MoSi 2 @Al 2 O 3 The suspension was placed in a thermostatically magnetically stirred water bath at a stirring speed of 800rpm and a temperature of 90 ℃. Adding yttrium nitrate solution into a separating funnel, and slowly dripping MoSi into the yttrium nitrate solution at a controlled speed 2 @Al 2 O 3 Suspending liquid, and dripping MoSi by sucking ammonia water with needle tube 2 @Al 2 O 3 The suspension was suspended to control the pH to 6. After the yttrium nitrate solution is completely dripped, the mixture is continuously stirred for 1 hour at constant temperature, and then is subjected to solid-liquid separation, washed by deionized water and subjected to solid-liquid separation. Drying the obtained solid in a drying box at 120 ℃ for 20h, and lightly grinding to obtain MoSi 2 @Al 2 O 3 @Y(OH) 3 And putting the powder into a vacuum tube furnace to be treated for 3 hours at 900 ℃, wherein the vacuum degree is less than 10Pa. Taking out and sieving to obtain MoSi 2 @Al 2 O 3 @Y 2 O 3 Self-healing powder with the upper and lower meshes of 150 meshes and 500 meshes.
Example 2
100 g of Al (NO) was added to 100ml of deionized water 3 ) 3 •9H 2 Preparing aluminum nitrate solution from O, and mixing 10g of MoSi with average particle size of 30-50 μm 2 The powder is dispersed in 200ml deionized water to prepare MoSi 2 And (3) suspension. Mixing MoSi 2 The suspension is placed in a constantIn the warm magnetic stirring water bath kettle, the stirring speed is 800rpm, and the temperature is 55 ℃. Adding the aluminum nitrate solution into a separating funnel, and slowly dripping MoSi into the aluminum nitrate solution at a controlled speed 2 Suspending liquid, and simultaneously sucking ammonia water by using a needle tube and dripping MoSi 2 The dispersion was controlled to pH 9.5. After the aluminum nitrate solution is completely dripped, the mixture is continuously stirred for 1 hour at constant temperature, and then solid-liquid separation is carried out, washing is carried out by using deionized water, and then solid-liquid separation is carried out. Drying the obtained solid in a drying box at 120 ℃ for 20h, and lightly grinding to obtain MoSi 2 @Al(OH) 3 And putting the powder into a vacuum tube furnace to be treated for 7 hours at 1200 ℃, wherein the vacuum degree is less than 10Pa. Taking out and sieving to obtain MoSi 2 @Al 2 O 3 The powder has 150-mesh and 500-mesh upper and lower meshes.
100 g of Y (NO) was added to 100ml of deionized water 3 ) 3 •6H 2 O into yttrium nitrate solution, 10g of MoSi 2 @Al 2 O 3 Dispersing in 200ml deionized water to prepare MoSi 2 @Al 2 O 3 (ii) a suspension. Mixing MoSi 2 @Al 2 O 3 The dispersion was placed in a constant temperature magnetic stirring water bath at a stirring speed of 800rpm and a temperature of 90 ℃. Putting yttrium nitrate solution into a separating funnel, and controlling the speed to slowly drop the yttrium nitrate solution into MoSi 2 @Al 2 O 3 Suspending liquid, and simultaneously sucking ammonia water by using a needle tube and dripping MoSi 2 @Y 2 O 3 The suspension was controlled to pH 7. After the yttrium nitrate solution is completely dripped into the solution, the solution is continuously stirred for 1 hour at constant temperature, then the solution is subjected to solid-liquid separation, the solution is washed by deionized water and then subjected to solid-liquid separation again, the solid matter is put into 400ml of absolute ethyl alcohol and stirred for 30min, and the solution is washed by the absolute ethyl alcohol and then subjected to solid-liquid separation. Drying the obtained solid in a drying box at 120 ℃ for 20h, and lightly grinding to obtain MoSi 2 @Al 2 O 3 @Y(OH) 3 Powder, which is put into a vacuum tube furnace to be treated at 900 ℃ for 5h and kept in a vacuum state (<10 Pa) is added. Taking out and sieving to obtain MoSi 2 @Al 2 O 3 @ Y 2 O 3 Self-healing powder with the upper and lower meshes of 150 meshes and 500 meshes.

Claims (3)

1. A kind ofThe preparation method of the self-healing powder with the double-shell structure is characterized by comprising the following steps of: the preparation method adopts MoSi 2 As a core material of self-healing powder, al (NO) 3 ) 3 •9H 2 O is an aluminum source, Y (NO) 3 ) 3 •6H 2 O is yttrium source, and Al is prepared as inner shell layer by two liquid phase precipitation and sintering 2 O 3 The outer shell layer is Y 2 O 3 Of MoSi 2 @Al 2 O 3 @Y 2 O 3 The self-healing powder comprises the following specific processes:
step 1: moSi 2 @Al 2 O 3 Preparation of the powder
At the temperature of 55 ℃, 1.5 to 2.5mol/L of Al (NO) is added under the condition of stirring 3 ) 3 The solution is dropwise added with MoSi of 50g/L 2 In the suspension, ammonia water is simultaneously dripped to control the pH value of the reaction system to be 8.5-9.5; after the dropwise addition of the materials is finished, continuously stirring and keeping the temperature for 1-2 hours;
carrying out solid-liquid separation on the reaction product, washing the obtained filter cake with deionized water for three times, placing the filter cake into absolute ethyl alcohol, stirring for 30min, carrying out solid-liquid separation, drying at 120 ℃ for 20h, grinding for 10 min, and sieving up and down by 150 meshes and 500 meshes to obtain MoSi 2 @Al(OH) 3 The powder is sintered for 3 to 7 hours in vacuum at 1200 ℃ and the vacuum degree of less than 10Pa, and then is sieved up and down by 150 meshes and 500 meshes to obtain MoSi 2 @Al 2 O 3 Powder;
and 2, step: moSi 2 @Al 2 O 3 @Y 2 O 3 Preparation of self-healing powders
At the temperature of 90 ℃, under the stirring condition, 1.5 to 2.5mol/L of Y (NO) is added 3 ) 3 The solution is dripped into 50g/L MoSi 2 @Al 2 O 3 The powder suspension is added with ammonia water dropwise to control the pH value of the reaction system to be 6-7; after the dropwise addition is finished, continuously stirring for 1 h;
carrying out solid-liquid separation on the reaction product, drying the obtained filter cake at 120 ℃ for 20h, and grinding for 10 min to obtain MoSi 2 @Al 2 O 3 @Y(OH) 3 The powder is then vacuumed at 900 deg.CSintering for 3-7 h, and sieving up and down by 150 meshes and 500 meshes to obtain the MoSi with the double-shell structure 2 @Al 2 O 3 @Y 2 O 3 Self-healing powder.
2. The method for preparing self-healing powder with double-shell structure according to claim 1, wherein: the MoSi 2 Has an average particle diameter of 30 to 50 μm.
3. The method for preparing self-healing powder with double-shell structure according to claim 1, wherein: the MoSi is 2 、Al(NO 3 ) 3 •9H 2 O、Y(NO 3 ) 3 •6H 2 The mass ratio of the dosage of the three raw materials of O is 1: 8-10.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090186237A1 (en) * 2008-01-18 2009-07-23 Rolls-Royce Corp. CMAS-Resistant Thermal Barrier Coatings
US20190284673A1 (en) * 2018-03-16 2019-09-19 Rolls-Royce Corporation Coating system including nucleating agent

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20090186237A1 (en) * 2008-01-18 2009-07-23 Rolls-Royce Corp. CMAS-Resistant Thermal Barrier Coatings
US20190284673A1 (en) * 2018-03-16 2019-09-19 Rolls-Royce Corporation Coating system including nucleating agent

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Creating a Protective Shell for Reactive MoSi2 Particles in High-Temperature Ceramics;Alexandra L. Carabat等;《Journal of the American Ceramic Society》;20150831;第98卷(第8期);第2609-2616 页 *

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