CN115354322B - Preparation method of high-pore thermal barrier coating - Google Patents
Preparation method of high-pore thermal barrier coating Download PDFInfo
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Abstract
A preparation method of a high-pore thermal barrier coating, which relates to a preparation method of a thermal barrier coating. In order to solve the problems of short service life and poor heat insulation effect of the thermal barrier coating prepared by the existing method, a preparation method of a high-pore thermal barrier coating is provided. The method comprises the following steps: preparing an intermediate connecting layer by using the surface of the electroplating matrix; preparing plasma spraying powder, and preparing a thermal barrier coating on the surface of the intermediate connecting layer by adopting a plasma spraying process; and carrying out heat treatment on the thermal barrier coating. The invention forms a core-shell structure by forming spray powder by soda lime glass and modified SiN ceramic micro powder, and introduces Fe 2 O 3 And a pore network is formed, so that the thermal conductivity and apparent elastic modulus of the thermal barrier coating are improved. The silicon oil generates free silicon atoms to repair and reconnect the defect, so that the structural integrity of SiN crystals is greatly improved.
Description
Technical Field
The invention relates to a preparation method of a thermal barrier coating.
Background
The steam turbine comprises a gas turbine, an aeroengine part and the like, and most of the gas turbine and the aeroengine part are made of high-temperature alloy materials with high-temperature strength, oxidation corrosion resistance and the like; the environment temperature of the internal parts of a general gas turbine and an aeroengine is about 1600 ℃, and the working limit of high-temperature alloys such as nickel-base single-crystal superalloy is far exceeded. In order to avoid the failure of the high-temperature alloy in the environment higher than the self temperature bearing limit, the preparation of the thermal barrier coating on the high-temperature alloy is one of the necessary heat insulation protection measures of the prior aeroengine and the ground combustion engine; the thermal barrier coating increases the temperature operating limit of the superalloy component.
The preparation method of the thermal barrier coating comprises a plasma spraying method, an electron beam physical vapor deposition method, a supersonic flame spraying method, an electrostatic spraying auxiliary vapor deposition method, a laser cladding method and the like, and the plasma spraying is a main preparation method of the thermal barrier coating. Plasma spraying can be a common primary manufacturing method. The patent with publication number CN114480999A discloses a super high temperature long service life thermal barrier coating material and a preparation method of the super high temperature long service life thermal barrier coating, wherein the super high temperature long service life thermal barrier coating is prepared by ball milling the super high temperature long service life thermal barrier coating material to obtain nano-aggregates, and spraying the nano-aggregates on a bonding layer to form a ceramic layer by an atmospheric plasma spraying process. The patent with publication number CN107815633A discloses a preparation method of a high-performance thermal barrier coating, which adopts a sol spray pyrolysis synthesis process to prepare 4YSZ powder with fine nano structure, uniform components and pure tetragonal phase, and then sequentially adopts spray drying granulation, screening and Atmospheric Plasma Spraying (APS) to prepare the coating.
Although plasma spraying has been widely used, increasing the service life of plasma sprayed thermal barrier coatings is a difficult problem that currently needs to be addressed. The high-temperature sintering of plasma spraying ensures that micropores in the coating heal in a large amount, the coating rigidity is improved, and the coating is too compact, so that the coating is extremely easy to crack after high-temperature service, the heat insulation effect of the coating is reduced, and the service life is shortened.
Disclosure of Invention
The invention provides a preparation method of a high-pore thermal barrier coating, which aims to solve the problems of short service life and poor heat insulation effect of the thermal barrier coating prepared by the existing method.
The preparation method of the high-pore thermal barrier coating comprises the following steps:
step one: carrying out surface impurity removal treatment on the high-temperature alloy matrix;
step two: preparing an intermediate connecting layer on the surface of the superalloy substrate by electroplating;
the intermediate connecting layer is made of Fe;
step three: preparing plasma spraying powder
(1) Placing polysilazane in a protective atmosphere and preserving heat for 0.4-0.5 h at 250-257 ℃ to obtain SiCN, crushing to obtain SiCN micro powder, and mixing with Fe 2 O 3 Mixing the micro powder, and then performing high-temperature pyrolysis to obtain SiN ceramic micro powder;
the Fe is 2 O 3 The addition amount of (2) is 5% of the mass of SiCN;
the high-temperature pyrolysis process comprises the following steps: sintering for 1.5h at 1180-1190 ℃ in nitrogen atmosphere;
(2) mixing the obtained SiN ceramic micro powder with silicone oil, and then sintering and ball milling to obtain modified SiN ceramic micro powder;
the sintering temperature is 500-620 ℃; the sintering time is 1-5 h;
the silicone oil is polyphenyl silicone oil, and the mass ratio of the silicone oil to the SiN ceramic micro powder is 0.2:1;
(3) grinding soda lime glass into micropowder, mixing with modified SiN ceramic micropowder, sintering, and ball milling to obtain spray powder;
the volume ratio of the soda lime glass to the modified SiN ceramic micro powder is (0.1-0.25) 1
Step four: preparing a thermal barrier coating with the thickness of 300-500 mu m on the surface of the intermediate connecting layer by adopting a plasma spraying process;
the plasma spraying process comprises the following steps: the spraying current is 400-500A, the spraying voltage is 45-55V, the powder feeding speed is 1-2.2 g/min, the argon flow is 90-120 SCFH, the hydrogen flow is 10-20 SCFH, the powder feeding direction is 90 degrees, the spraying distance is 400-500 mm, and the spraying speed is 20mm/s;
fifthly, performing heat treatment on the thermal barrier coating to finish the process;
the heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1000-1200 ℃, the heat preservation time is 10-15 h, and the heating rate is 10-15 ℃/min.
The principle and beneficial effects of the invention are as follows:
according to the invention, a thermal barrier coating is formed on the surface of a nickel-based single crystal superalloy substrate after plasma spraying, in spraying powder composed of soda lime glass and modified SiN ceramic micropowder, the softening point of the soda lime glass is low, the effect of bonding and separating modified SiN ceramic micropowder particles is achieved in the preparation of the thermal barrier middle coating, the modified SiN ceramic micropowder is stacked to form a network structure in the plasma spraying process, and the SiN ceramic micropowder is coated with the soda lime glass to form a core-shell structure; fe in SiCN 2 O 3 Is excessive, namely a catalyst and a pore-forming agent; soda lime glass forms a melt during plasma spraying, fe 2 O 3 Oxygen generated by decomposition at high temperature escapes into the soda-lime glass melt to form pores, and excessive oxygen flows to the outside of the thermal barrier coating to form longitudinal pores perpendicular to the heat flow direction, and the pores and the longitudinal pores form a pore network, so that the thermal conductivity and apparent elastic modulus of the thermal barrier coating are improved. According to the invention, the silicone oil is decomposed into short-chain siloxane after sintering to generate free silicon atoms, silicon diffuses into SiN ceramic at high temperature to occupy defect sites of SiN, and repair and reconnection are carried out on the defect sites, so that the structural integrity of SiN crystals is greatly improved. The intermediate connecting layer is made of Fe, and is used for gradient transition of linear expansion performance between the high-temperature alloy matrix and the thermal barrier coating, so that the thermal stability of the joint is ensured. Fe in the intermediate connecting layer material and Fe in the thermal barrier coating are mutually diffused at high temperature to form a new interface product, so that the interface binding force between the high-temperature alloy matrix and the thermal barrier coating is improved, and the thermal barrier coating is prevented from cracking and peeling after high-temperature service.
Drawings
FIG. 1 is a photomicrograph of the high porosity thermal barrier coating prepared in example 1;
Detailed Description
The technical scheme of the invention is not limited to the specific embodiments listed below, and also comprises any reasonable combination of the specific embodiments.
The first embodiment is as follows: step one of this embodiment: carrying out surface impurity removal treatment on the high-temperature alloy matrix;
step two: preparing an intermediate connecting layer on the surface of the superalloy substrate by electroplating;
the intermediate connecting layer is made of Fe;
step three: preparing plasma spraying powder
(1) Placing polysilazane in a protective atmosphere and preserving heat for 0.4-0.5 h at 250-257 ℃ to obtain SiCN, crushing to obtain SiCN micro powder, and mixing with Fe 2 O 3 Mixing the micro powder, and then performing high-temperature pyrolysis to obtain SiN ceramic micro powder;
the Fe is 2 O 3 The addition amount of (2) is 5% of the mass of SiCN;
the high-temperature pyrolysis process comprises the following steps: sintering for 1.5h at 1180-1190 ℃ in nitrogen atmosphere;
(2) mixing the obtained SiN ceramic micro powder with silicone oil, and then sintering and ball milling to obtain modified SiN ceramic micro powder;
the sintering temperature is 500-620 ℃; the sintering time is 1-5 h;
the silicone oil is polyphenyl silicone oil, and the mass ratio of the silicone oil to the SiN ceramic micro powder is 0.2:1;
(3) grinding soda lime glass into micropowder, mixing with modified SiN ceramic micropowder, sintering, and ball milling to obtain spray powder;
the volume ratio of the soda lime glass to the modified SiN ceramic micro powder is (0.1-0.25) 1
Step four: preparing a thermal barrier coating with the thickness of 300-500 mu m on the surface of the intermediate connecting layer by adopting a plasma spraying process;
the plasma spraying process comprises the following steps: the spraying current is 400-500A, the spraying voltage is 45-55V, the powder feeding speed is 1-2.2 g/min, the argon flow is 90-120 SCFH, the hydrogen flow is 10-20 SCFH, the powder feeding direction is 90 degrees, the spraying distance is 400-500 mm, and the spraying speed is 20mm/s;
fifthly, performing heat treatment on the thermal barrier coating to finish the process;
the heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1000-1200 ℃, the heat preservation time is 10-15 h, and the heating rate is 10-15 ℃/min.
The present embodiment has the following advantageous effects:
in the embodiment, after plasma spraying, a thermal barrier coating is formed on the surface of a nickel-based single crystal superalloy substrate, in spraying powder consisting of soda lime glass and modified SiN ceramic micropowder, the softening point of the soda lime glass is low, the effect of bonding and separating modified SiN ceramic micropowder particles is achieved in the preparation of the thermal barrier middle coating, the modified SiN ceramic micropowder is stacked to form a network structure in the plasma spraying process, and the SiN ceramic micropowder coats the soda lime glass to form a core-shell structure; fe in SiCN 2 O 3 Is excessive, namely a catalyst and a pore-forming agent; soda lime glass forms a melt during plasma spraying, fe 2 O 3 Oxygen generated by decomposition at high temperature escapes into the soda-lime glass melt to form pores, and excessive oxygen flows to the outside of the thermal barrier coating to form longitudinal pores perpendicular to the heat flow direction, and the pores and the longitudinal pores form a pore network, so that the thermal conductivity and apparent elastic modulus of the thermal barrier coating are improved. In the embodiment, the silicone oil is decomposed into short-chain siloxane after sintering to generate free silicon atoms, silicon diffuses into SiN ceramic at high temperature to occupy defect sites of SiN, and the defect sites are repaired and reconnected, so that the structural integrity of SiN crystals is greatly improved. The intermediate connecting layer adopted in the embodiment is made of Fe, and is used for gradient transition of linear expansion performance between the high-temperature alloy matrix and the thermal barrier coating, so that the thermal stability of the joint is ensured. Fe in the intermediate connecting layer material and Fe in the thermal barrier coating are mutually diffused at high temperature to form a new interface product, so that the interface binding force between the high-temperature alloy matrix and the thermal barrier coating is improved, and the thermal barrier coating is prevented from cracking and peeling after high-temperature service.
The second embodiment is as follows: the first difference between this embodiment and the specific embodiment is that: the superalloy substrate is nickel-based single crystal superalloy.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the surface impurity removal treatment process is sand blasting.
The specific embodiment IV is as follows: this embodiment differs from one of the first to third embodiments in that: and step two, the thickness of the intermediate connecting layer is 1-50 mu m.
Fifth embodiment: this embodiment differs from one to four embodiments in that: and step three, the particle size of the SiCN micro powder is 20-30 mu m.
Specific embodiment six: this embodiment differs from one of the first to fifth embodiments in that: step three, fe 2 O 3 The grain size of the micro powder is 20-30 mu m.
Seventh embodiment: this embodiment differs from one of the first to sixth embodiments in that: and (3) the protective atmosphere in the step (1) is nitrogen, helium or argon.
Eighth embodiment: this embodiment differs from one of the first to seventh embodiments in that: and step three, the particle size of the spraying powder is 30-60 mu m.
Detailed description nine: this embodiment differs from one to eight of the embodiments in that: and step four, the plasma spraying process comprises the following steps: the spraying current is 450A, the spraying voltage is 50V, the powder feeding speed is 2g/min, the argon flow is 90SCFH, the hydrogen flow is 15SCFH, the powder feeding direction is 90 degrees, the spraying distance is 500mm, and the spraying speed is 20mm/s.
Detailed description ten: this embodiment differs from one of the embodiments one to nine in that: the heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1100 ℃, the heat preservation time is 12 hours, and the heating rate is 12 ℃/min.
Example 1:
the preparation method of the high-porosity thermal barrier coating comprises the following steps:
step one: surface impurity removal treatment is carried out on the substrate;
the matrix is nickel-based single crystal superalloy (DD 403);
the surface impurity removal treatment process is sand blasting;
step two: preparing an intermediate connecting layer on the surface of the superalloy substrate by electroplating;
the intermediate connecting layer is made of Fe;
the thickness of the intermediate connecting layer is 5 mu m;
step three: preparing plasma spraying powder
(1) Placing polysilazane in protective atmosphere and keeping the temperature at 250 ℃ for 0.5h to obtain SiCN, crushing to obtain SiCN micropowder, and mixing with Fe 2 O 3 Mixing the micro powder, and then performing high-temperature pyrolysis to obtain SiN ceramic micro powder;
the Fe is 2 O 3 The addition amount of (2) is 5% of the mass of SiCN;
the particle size of the SiCN micro powder is 25 mu m;
the Fe is 2 O 3 The grain diameter of the micro powder is 25 mu m;
the high-temperature pyrolysis process comprises the following steps: sintering for 1.5h at 1190 ℃ in nitrogen atmosphere;
the protective atmosphere in the third step (1) is nitrogen, helium or argon;
(2) mixing the obtained SiN ceramic micro powder with silicone oil, and then sintering and ball milling to obtain modified SiN ceramic micro powder;
the sintering temperature is 600 ℃; the sintering time is 4 hours;
the silicone oil is polyphenyl silicone oil, and the mass ratio of the silicone oil to the SiN ceramic micro powder is 0.2:1;
(3) grinding soda lime glass into micropowder, mixing with modified SiN ceramic micropowder, sintering, and ball milling to obtain spray powder;
the particle size of the spraying powder is 40 mu m;
the volume ratio of the soda lime glass to the modified SiN ceramic micro powder is 0.1:1
Step four: preparing a thermal barrier coating with the thickness of 400 mu m on the surface of the intermediate connecting layer by adopting a plasma spraying process;
the plasma spraying process comprises the following steps: the spraying current is 450A, the spraying voltage is 50V, the powder feeding speed is 2g/min, the argon flow is 90SCFH, the hydrogen flow is 15SCFH, the powder feeding direction is 90 degrees, the spraying distance is 500mm, and the spraying speed is 20mm/s.
And fifthly, performing heat treatment on the thermal barrier coating to finish the process.
The heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1100 ℃, the heat preservation time is 12 hours, and the heating rate is 12 ℃/min.
FIG. 1 is a photomicrograph of the high porosity thermal barrier coating prepared in example 1; fig. 1 shows that the thermal barrier coating contains longitudinal pores, and the pores are rich, so that a pore network is formed. According to the test of the thermal spraying coating bonding strength test method (HB 5476-91), the interface bonding strength of the thermal barrier coating obtained in the embodiment reaches 95MPa.
Example 2:
the preparation method of the high-porosity thermal barrier coating comprises the following steps:
step one: surface impurity removal treatment is carried out on the substrate;
the matrix is nickel-based single crystal superalloy (DD 403); the surface impurity removal treatment process is sand blasting;
step two: preparing an intermediate connecting layer on the surface of the superalloy substrate by electroplating;
the intermediate connecting layer is made of Fe; the thickness of the intermediate connecting layer is 10 mu m;
step three: preparing plasma spraying powder
(1) Placing polysilazane in protective atmosphere and keeping the temperature at 250 ℃ for 0.4h to obtain SiCN, crushing to obtain SiCN micropowder, and mixing with Fe 2 O 3 Mixing the micro powder, and then performing high-temperature pyrolysis to obtain SiN ceramic micro powder;
the Fe is 2 O 3 The addition amount of (2) is 5% of the mass of SiCN;
the particle size of the SiCN micro powder is 25 mu m;
the Fe is 2 O 3 The grain diameter of the micro powder is 25 mu m;
the high-temperature pyrolysis process comprises the following steps: sintering for 1.5h at 1180 ℃ in nitrogen atmosphere;
the protective atmosphere in the third step (1) is nitrogen, helium or argon;
(2) mixing the obtained SiN ceramic micro powder with silicone oil, and then sintering and ball milling to obtain modified SiN ceramic micro powder;
the sintering temperature is 550 ℃; the sintering time is 4 hours;
the silicone oil is polyphenyl silicone oil, and the mass ratio of the silicone oil to the SiN ceramic micro powder is 0.2:1;
(3) grinding soda lime glass into micropowder, mixing with modified SiN ceramic micropowder, sintering, and ball milling to obtain spray powder;
the particle size of the spraying powder is 40 mu m;
the volume ratio of the soda lime glass to the modified SiN ceramic micro powder is 0.1:1
Step four: preparing a thermal barrier coating with the thickness of 400 mu m on the surface of the intermediate connecting layer by adopting a plasma spraying process;
the plasma spraying process comprises the following steps: the spraying current is 450A, the spraying voltage is 50V, the powder feeding speed is 2g/min, the argon flow is 90SCFH, the hydrogen flow is 15SCFH, the powder feeding direction is 90 degrees, the spraying distance is 500mm, and the spraying speed is 20mm/s.
And fifthly, performing heat treatment on the thermal barrier coating to finish the process.
The heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1100 ℃, the heat preservation time is 12 hours, and the heating rate is 12 ℃/min.
The interface bonding strength of the thermal barrier coating obtained in the embodiment reaches 92MPa. The thermal barrier coating obtained in the embodiment has only tiny black spots on the surface of the sample after 1000 times of flame (1500 ℃) thermal shock, and no spalling and cracking are found.
Claims (10)
1. A preparation method of a high-porosity thermal barrier coating is characterized by comprising the following steps: the preparation method of the high-pore thermal barrier coating comprises the following steps:
step one: carrying out surface impurity removal treatment on the high-temperature alloy matrix;
step two: preparing an intermediate connecting layer on the surface of the superalloy substrate by electroplating;
the intermediate connecting layer is made of Fe;
step three: preparing plasma spraying powder
(1) Placing polysilazane in a protective atmosphere and preserving heat for 0.4-0.5 h at 250-257 ℃ to obtain SiCN, crushing to obtain SiCN micro powder, and mixing with Fe 2 O 3 Mixing the micro powder, and then performing high-temperature pyrolysis to obtain SiN ceramic micro powder;
the Fe is 2 O 3 The addition amount of (2) is 5% of the mass of SiCN;
the high-temperature pyrolysis process comprises the following steps: sintering for 1.5h at 1180-1190 ℃ in nitrogen atmosphere;
(2) mixing the obtained SiN ceramic micro powder with silicone oil, and then sintering and ball milling to obtain modified SiN ceramic micro powder;
the sintering temperature is 500-620 ℃; the sintering time is 1-5 h;
the silicone oil is polyphenyl silicone oil, and the mass ratio of the silicone oil to the SiN ceramic micro powder is 0.2:1;
(3) grinding soda lime glass into micropowder, mixing with modified SiN ceramic micropowder, sintering, and ball milling to obtain spray powder;
the volume ratio of the soda lime glass to the modified SiN ceramic micro powder is (0.1-0.25) 1
Step four: preparing a thermal barrier coating with the thickness of 300-500 mu m on the surface of the intermediate connecting layer by adopting a plasma spraying process;
the plasma spraying process comprises the following steps: the spraying current is 400-500A, the spraying voltage is 45-55V, the powder feeding speed is 1-2.2 g/min, the argon flow is 90-120 SCFH, the hydrogen flow is 10-20 SCFH, the powder feeding direction is 90 degrees, the spraying distance is 400-500 mm, and the spraying speed is 20mm/s;
fifthly, performing heat treatment on the thermal barrier coating to finish the process;
the heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1000-1200 ℃, the heat preservation time is 10-15 h, and the heating rate is 10-15 ℃/min.
2. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: the superalloy substrate is nickel-based single crystal superalloy.
3. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: the surface impurity removal treatment process is sand blasting.
4. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: and step two, the thickness of the intermediate connecting layer is 1-50 mu m.
5. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: and step three, the particle size of the SiCN micro powder is 20-30 mu m.
6. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: step three, fe 2 O 3 The grain size of the micro powder is 20-30 mu m.
7. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: and (3) the protective atmosphere in the step (1) is nitrogen, helium or argon.
8. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: and step three, the particle size of the spraying powder is 30-60 mu m.
9. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: and step four, the plasma spraying process comprises the following steps: the spraying current is 450A, the spraying voltage is 50V, the powder feeding speed is 2g/min, the argon flow is 90SCFH, the hydrogen flow is 15SCFH, the powder feeding direction is 90 degrees, the spraying distance is 500mm, and the spraying speed is 20mm/s.
10. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: the heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1100 ℃, the heat preservation time is 12 hours, and the heating rate is 12 ℃/min.
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