CN115354322A - Preparation method of high-porosity thermal barrier coating - Google Patents
Preparation method of high-porosity thermal barrier coating Download PDFInfo
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Abstract
A preparation method of a high-porosity thermal barrier coating 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 the high-porosity thermal barrier coating is provided. The method comprises the following steps: preparing an intermediate connecting layer on the surface of an electroplating substrate; 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 relates to soda-lime glass and modified SiNThe ceramic micro powder forms spraying powder to form a core-shell structure, and Fe is introduced 2 O 3 A pore network is formed, and the thermal conductivity and the apparent elastic modulus of the thermal barrier coating are improved. The silicon oil generates free silicon atoms to repair and reconnect the defect position, so that the structural integrity of the crystal of the SiN is greatly improved, the interface bonding force between the high-temperature alloy matrix and the thermal barrier coating is high, and the thermal barrier coating is prevented from cracking and peeling after high-temperature service.
Description
Technical Field
The invention relates to a preparation method of a thermal barrier coating.
Background
The steam turbine comprises a gas turbine, an aircraft engine part and the like, and most of the gas turbine and the aircraft engine part are high-temperature alloy materials with high-temperature strength, oxidation and corrosion resistance and the like; the environmental temperature of the internal parts of the general gas turbine and the aircraft engine is about 1600 ℃, which far exceeds the working limit of high-temperature alloys such as nickel-based single crystal superalloy and the like. 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 protective measures of the current aeroengine and ground combustion engine; thermal barrier coatings increase the temperature operating limit of superalloy components.
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, wherein the plasma spraying is a main preparation method of the thermal barrier coating. Plasma spraying can be the common primary method of preparation. The patent publication No. CN114480999A discloses an ultrahigh-temperature long-life thermal barrier coating material and a preparation method of the ultrahigh-temperature long-life thermal barrier coating, wherein the ultrahigh-temperature long-life thermal barrier coating is prepared by ball-milling the ultrahigh-temperature long-life thermal barrier coating material to obtain nano aggregates, and spraying the nano aggregates on a bonding layer by an atmospheric plasma spraying process to form a ceramic layer. 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 prepares the coating by spray drying granulation, screening and Atmospheric Plasma Spraying (APS) in sequence.
Although the plasma spraying method is widely applied, the service life of the thermal barrier coating of the plasma spraying is a difficult problem which needs to be solved at present. The high-temperature sintering of plasma spraying enables a large number of micropores in the coating to be healed, the rigidity of the coating is improved, and the coating is too compact, so that the coating is 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-porosity thermal barrier coating, aiming at solving 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-porosity thermal barrier coating is carried out according to the following steps:
the method comprises the following steps: carrying out surface impurity removal treatment on the high-temperature alloy matrix;
step two: preparing an intermediate connecting layer on the surface of the high-temperature alloy substrate by electroplating;
the middle connecting layer is made of Fe;
step three: preparation of plasma spray powder
(1) Placing polysilazane in protective atmosphere and keeping the temperature at 250-257 ℃ for 0.4-0.5 h to obtain SiCN, crushing to obtain SiCN micro powder, mixing with Fe 2 O 3 Mixing the micro powders, and then carrying out high-temperature pyrolysis to obtain SiN ceramic micro powder;
said Fe 2 O 3 The addition amount of (A) 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;
(3) grinding soda-lime glass into micro powder, mixing the micro powder with the modified SiN ceramic micro powder, sintering, and performing ball milling after sintering to obtain spraying 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 middle 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;
step five, carrying out heat treatment on the thermal barrier coating to finish the process;
the thermal 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 the beneficial effects of the invention are as follows:
after plasma spraying, a thermal barrier coating is formed on the surface of a nickel-based single crystal high-temperature alloy substrate, in the spraying powder consisting of soda-lime glass and modified SiN ceramic micro powder, the softening point of the soda-lime glass is low, the coating plays a role in bonding and separating modified SiN ceramic micro powder particles in the preparation of the thermal barrier middle coating, the modified SiN ceramic micro powder is stacked to form a network structure in the plasma spraying process, and the SiN ceramic micro powder covers the soda-lime glass to form a core-shell structure; fe in SiCN 2 O 3 Is excessive, i.e. is a catalyst and is also a pore-forming agent; the soda-lime glass forms a melt, fe, during plasma spraying 2 O 3 The oxygen generated by decomposition at high temperature escapes into the soda-lime glass melt to form air holes, and meanwhile, the excessive oxygen flows to the outside of the thermal barrier coating to form longitudinal pores perpendicular to the heat flow direction, and the air holes and the longitudinal pores form a pore network, so that the heat conductivity and the apparent elastic modulus of the thermal barrier coating are improved. According to the invention, silicone oil is decomposed into short-chain siloxane after sintering, free silicon atoms are generated, silicon is diffused into SiN ceramic to occupy SiN defect sites at high temperature, and the defect sites are repaired and reconnected, so that the structural integrity of SiN crystals is greatly improved. The intermediate connecting layer adopted by the invention is made of Fe and is used for gradient transition of linear expansion performance between the high-temperature alloy substrate and the thermal barrier coating, so that the thermal stability of the joint is ensured. Fe in the material of the intermediate connecting layer and Fe in the thermal barrier coating diffuse mutually at high temperature to form a new interface product, so that the interface bonding force between the high-temperature alloy substrate 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 a 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 any reasonable combination of the specific embodiments is included.
The first embodiment is as follows: the first step of the present 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 high-temperature alloy substrate by electroplating;
the middle connecting layer is made of Fe;
step three: preparation of plasma spray powder
(1) Placing polysilazane in protective atmosphere and keeping the temperature at 250-257 ℃ for 0.4-0.5 h to obtain SiCN, crushing to obtain SiCN micro powder, mixing with Fe 2 O 3 Mixing the micro powders, and then carrying out high-temperature pyrolysis to obtain SiN ceramic micro powder;
said Fe 2 O 3 The addition amount of (A) 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;
(3) grinding soda-lime glass into micro powder, mixing the micro powder with the modified SiN ceramic micro powder, sintering, and performing ball milling after sintering to obtain spraying powder;
the volume ratio of the soda-lime glass to the modified SiN ceramic micro powder is (0.1-0.25) to 1
Step four: preparing a thermal barrier coating with the thickness of 300-500 mu m on the surface of the middle 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;
step five, carrying out heat treatment on the thermal barrier coating to finish the process;
the thermal 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 embodiment has the following beneficial effects:
after plasma spraying, a thermal barrier coating is formed on the surface of a nickel-based single-crystal high-temperature alloy substrate, and in the spraying powder consisting of soda-lime glass and modified SiN ceramic micro powder, the softening point of the soda-lime glass is low, so that the coating plays a role in adhering and separating modified SiN ceramic micro powder particles in preparing the thermal barrier coating, the modified SiN ceramic micro powder is stacked to form a network structure in the plasma spraying process, and the SiN ceramic micro powder covers the soda-lime glass to form a core-shell structure; fe in SiCN 2 O 3 Is excessive, i.e. is a catalyst and is also a pore-forming agent; the soda-lime glass forms a melt, fe, during plasma spraying 2 O 3 The thermal barrier coating is decomposed at high temperature to generate oxygen which escapes into the soda-lime glass melt to form air holes, meanwhile, excessive oxygen flows to the outside of the thermal barrier coating to form longitudinal holes perpendicular to the heat flow direction, and the air holes and the longitudinal holes form a hole network, so that the thermal conductivity and the 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, the silicon is diffused into the SiN ceramic at high temperature to occupy SiN defect sites, and the defect sites are repaired and reconnected, so that the structural integrity of the SiN crystal is greatly improved. The intermediate connecting layer adopted by the embodiment is made of Fe, and is used for gradient transition of linear expansion performance between the high-temperature alloy substrate and the thermal barrier coating to ensure connectionThermal stability of the head. Fe in the material of the intermediate connecting layer and Fe in the thermal barrier coating diffuse mutually at high temperature to form a new interface product, so that the interface bonding force between the high-temperature alloy substrate 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 the present embodiment and the specific embodiment is: step one, the high-temperature alloy substrate is nickel-based single crystal high-temperature alloy.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: step one, the surface impurity removal treatment process is sand blasting.
The fourth concrete implementation mode is as follows: the difference between this embodiment and one of the first to third embodiments is: and step two, the thickness of the intermediate connecting layer is 1-50 mu m.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and step three, the particle size of the SiCN micro powder is 20-30 mu m.
The sixth specific implementation mode is as follows: the difference between this embodiment and one of the first to fifth embodiments is: step three of Fe 2 O 3 The particle size of the micro powder is 20-30 μm.
The seventh concrete implementation mode: the difference between this embodiment and one of the first to sixth embodiments is: and the protective atmosphere in the step three (1) is nitrogen, helium or argon.
The specific implementation mode eight: the present embodiment differs from one of the first to seventh embodiments in that: and the particle size of the spraying powder in the third step (3) is 30-60 mu m.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: 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.
The specific implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments 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 12h, and the heating rate is 12 ℃/min.
Example 1:
the preparation method of the high-porosity thermal barrier coating of the embodiment comprises the following steps:
the method comprises the following steps: carrying out surface impurity removal treatment on the substrate;
the substrate 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 high-temperature alloy substrate by electroplating;
the middle connecting layer is made of Fe;
the thickness of the middle connecting layer is 5 mu m;
step three: preparation of plasma spray powder
(1) Placing polysilazane in protective atmosphere and keeping the temperature at 250 ℃ for 0.5h to obtain SiCN, crushing to obtain SiCN micro powder, mixing with Fe 2 O 3 Mixing the micro powder, and then carrying out high-temperature pyrolysis to obtain SiN ceramic micro powder;
said Fe 2 O 3 The addition amount of (A) is 5% of the mass of SiCN;
the particle size of the SiCN micro powder is 25 mu m;
said Fe 2 O 3 The particle size of the micro powder is 25 μm;
the high-temperature pyrolysis process comprises the following steps: sintering for 1.5h at 1190 ℃ in the nitrogen atmosphere;
the protective atmosphere in the step three (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 4h;
the silicone oil is polyphenyl silicone oil, and the mass ratio of the silicone oil to the SiN ceramic micro powder is 0.2;
(3) grinding soda-lime glass into micro powder, mixing the micro powder with the modified SiN ceramic micro powder, sintering, and performing ball milling after sintering to obtain spraying 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
Step four: preparing a thermal barrier coating with the thickness of 400 mu m on the surface of the middle 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 thermal treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1100 ℃, the heat preservation time is 12h, and the heating rate is 12 ℃/min.
FIG. 1 is a photomicrograph of a high porosity thermal barrier coating prepared in example 1; FIG. 1 shows that the thermal barrier coating contains longitudinal pores, which are abundant and form a pore network. According to the test of the bonding strength test method of the thermal spraying coating (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 of the embodiment is carried out according to the following steps:
the method comprises the following steps: carrying out surface impurity removal treatment on the substrate;
the substrate 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 high-temperature alloy substrate by electroplating;
the middle connecting layer is made of Fe; the thickness of the middle connecting layer is 10 mu m;
step three: preparation of plasma spray powder
(1) Placing polysilazane in protective atmosphere and keeping the temperature at 250 ℃ for 0.4h to obtain SiCN, crushing to obtain SiCN micro powder, mixing with Fe 2 O 3 Mixing the micro powder, and then carrying out high-temperature pyrolysis to obtain SiN ceramic micro powder;
said Fe 2 O 3 The addition amount of (A) is 5% of the mass of SiCN;
the particle size of the SiCN micro powder is 25 mu m;
said Fe 2 O 3 The particle size of the micro powder is 25 μm;
the high-temperature pyrolysis process comprises the following steps: sintering for 1.5h at 1180 ℃ in nitrogen atmosphere;
the protective atmosphere in the step three (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 4h;
the silicone oil is polyphenyl silicone oil, and the mass ratio of the silicone oil to the SiN ceramic micro powder is 0.2;
(3) grinding soda-lime glass into micro powder, mixing the micro powder with the modified SiN ceramic micro powder, sintering, and performing ball milling after sintering to obtain spraying 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
Step four: preparing a thermal barrier coating with the thickness of 400 mu m on the surface of the middle 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 thermal treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1100 ℃, the heat preservation time is 12h, and the heating rate is 12 ℃/min.
The interface bonding strength of the thermal barrier coating obtained by the embodiment reaches 92MPa. The thermal barrier coating obtained in the embodiment has only tiny black spots on the surface of the test sample after being subjected to thermal shock of 1000 times of flame (1500 ℃), and has no spalling and cracking.
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-porosity thermal barrier coating is carried out according to the following steps:
the method comprises the following steps: carrying out surface impurity removal treatment on the high-temperature alloy matrix;
step two: preparing an intermediate connecting layer on the surface of the high-temperature alloy substrate by electroplating;
the middle connecting layer is made of Fe;
step three: preparation of plasma spray powder
(1) Placing polysilazane in protective atmosphere and keeping the temperature at 250-257 ℃ for 0.4-0.5 h to obtain SiCN, crushing to obtain SiCN micro powder, mixing with Fe 2 O 3 Mixing the micro powders, and then carrying out high-temperature pyrolysis to obtain SiN ceramic micro powder;
said Fe 2 O 3 The addition amount of (A) 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;
(3) grinding soda-lime glass into micro powder, mixing the micro powder with the modified SiN ceramic micro powder, sintering, and performing ball milling after sintering to obtain spraying 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 middle 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;
step five, carrying out heat treatment on the thermal barrier coating to finish the process;
the thermal 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: step one, the high-temperature alloy substrate is nickel-based single crystal high-temperature alloy.
3. The method of preparing a high porosity thermal barrier coating of claim 1, wherein: step one, 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 of claim 1, wherein: step three of Fe 2 O 3 The particle size of the micro powder is 20-30 μm.
7. The method of preparing a high porosity thermal barrier coating according to claim 1, characterized in that: and (2) the protective atmosphere in the step three (1) is nitrogen, helium or argon.
8. The method of preparing a high porosity thermal barrier coating of claim 1, wherein: and the particle size of the spraying powder in the third step (3) is 30-60 mu m.
9. The method of preparing a high porosity thermal barrier coating of claim 1, wherein: 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: fifthly, the heat treatment process of the thermal barrier coating comprises the following steps: the heat treatment temperature is 1100 ℃, the heat preservation time is 12h, and the heating rate is 12 ℃/min.
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