CN115466114A - High-toughness long-life ultrahigh-temperature thermal barrier coating material and preparation method and application thereof - Google Patents
High-toughness long-life ultrahigh-temperature thermal barrier coating material and preparation method and application thereof Download PDFInfo
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- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B64—AIRCRAFT; AVIATION; COSMONAUTICS
- B64D—EQUIPMENT FOR FITTING IN OR TO AIRCRAFT; FLIGHT SUITS; PARACHUTES; ARRANGEMENTS OR MOUNTING OF POWER PLANTS OR PROPULSION TRANSMISSIONS IN AIRCRAFT
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
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Abstract
The invention provides a thermal barrier coating material and a preparation method and application thereof, belonging to the technical field of ultrahigh-temperature protective coatings of aircraft engines and gas turbines. The invention takes the rare earth zirconate crystal structure as the target, fully considers the requirements of infrared radiation, high thermal expansion coefficient, low thermal conductivity and high fracture toughness of overtemperature service, and passes through Gd 3+ 、Sm 3+ And Yb 3+ The ternary rare earth reconstructs pyrochlore crystal structure, the proportion of the components is regulated and controlled, the defect concentration of the crystal is increased, and Yb is used 3+ The substitution of the material enhances the lattice distortion, effectively reduces the high-temperature infrared radiation heat transfer, and on the basis of ensuring the low thermal conductivity and high thermal expansion coefficient of the material, high fracture toughness and excellent high temperature resistance are realized, and the service life of the coating is further prolonged. By Ce of the invention 4+ For part of Zr 4+ Or Hf 4+ The substitution of crystal lattice positions further increases the defect concentration of the whole crystal, reduces the thermal conductivity of the material, and improves the performances of corrosion resistance, high temperature resistance, fracture toughness and the like.
Description
Technical Field
The invention relates to the technical field of ultrahigh-temperature protective coatings of aero-engines and gas turbines, in particular to a high-toughness long-life ultrahigh-temperature thermal barrier coating material and a preparation method and application thereof.
Background
The thermal barrier coating has wide and important application on the surfaces of high-temperature hot end parts of aeroengines and gas turbines (two-machine), and is a key technology for continuously improving the inlet temperature of the turbine and prolonging the service life and comprehensive performance of the hot end parts. 6 to 8wt.% Y 2 O 3 Partially stabilized ZrO 2 The (YSZ) thermal barrier coating is easy to generate phase change at high temperature and is accompanied by about 4 percent of volume expansion, the Young modulus of the coating is increased and the strain tolerance is reduced due to accelerated sintering, the thermal cycle life is shortened, and the long-time working temperature is lower than 1200 ℃. With the continuous development of the 'two-machine' technology, the highest temperature of the turbine inlet breaks through 1800 ℃, and the development of a novel high-toughness and long-service-life ultra-high-temperature thermal barrier coating with the use temperature of 1400-1600 ℃ becomes a key problem to be broken through urgently in the heat insulation protection of a new generation 'two-machine' high-temperature hot end component in consideration of the air film cooling design and the service working condition of a special part.
Because the YSZ thermal barrier coating can not meet the development requirement of a new generation of 'two machines', a large number of novel ultrahigh-temperature thermal barrier coating materials are researched at home and abroad in the past two decades, and the novel ultrahigh-temperature thermal barrier coating materials mainly comprise the following types:
(1) Pyrochlore structure rare earth zirconate Re 2 Zr 2 O 7 The thermal barrier coating material (Re = La, nd, sm, eu and Gd) has low thermal conductivity, no phase change at room temperature to 1550 ℃, and a thermal expansion coefficient of 9 to 12 multiplied by 10 -6 K -1 . However, such materials have low fracture toughness and short thermal cycle life of single-layer coatings. In addition, a single pyrochlore rare earth zirconate coating is susceptible to high temperature chemical reaction with the thermally grown oxide TGO. E.g. pyrochlore structure Gd with highest coefficient of thermal expansion 2 Zr 2 O 7 Is not suitable to be used as a single thermal barrier ceramic layer directly on the surface of the metal bonding layer.
(2) A multi-element rare earth co-doped YSZ-based high-temperature thermal barrier coating material. YSZ has the best thermo-mechanical matching property with a metal substrate, and by means of multi-element rare earth doping, tetragonal YSZ (with proper amount of rare earth elements co-doped and still maintaining tetragonal crystal structure) or cubic YSZ (with the total doping amount of various rare earth elements including Y being about 20 wt.%) with high crystal defects is formed, so that the thermal conductivity of the material is reduced, high fracture toughness and thermal expansion coefficient are ensured, and no phase change exists between room temperature and 1600 ℃. However, researches show that the YSZ-based multi-element rare earth doped modified thermal barrier coating material can still be rapidly sintered at the temperature of more than or equal to 1500 ℃, the strain tolerance and the high-temperature thermal cycle life of the material are greatly reduced, and the requirements of a new generation of 'two machines' on the development of ultra-high temperature thermal barrier coatings cannot be met.
(3) Although the high-temperature phase stability of the rare earth tantalate and rare earth niobate thermal barrier coating materials is good, the raw material cost is high, the fracture toughness is relatively low, and the thermal cycle life of the thermal barrier coating at the ultrahigh temperature of 1400-1600 ℃ and the use of the thermal barrier coating on hot end parts of two machines are limited.
Further, la 2 Ce 2 O 7 、La 2 (Zr 0.7 Ce 0.3 ) 2 O 7 The novel thermal barrier coating materials such as the magnetoplumbite structure rare earth hexaaluminate have no phase change from room temperature to 1600 ℃, but have the problems of deviation of stoichiometric ratio or large amorphous phase content, or high ultrahigh temperature sintering rate and the like in the coating preparation process, and the ultrahigh temperature service reliability of the coating needs to be further researched and demonstrated.
Therefore, the novel high-toughness and long-service-life ultrahigh-temperature thermal barrier coating material with the use temperature of 1400-1600 ℃ still remains a key problem to be solved for developing a new generation of high-performance thermal barrier coating material.
Disclosure of Invention
The invention aims to provide a high-toughness long-life ultrahigh-temperature thermal barrier coating material, and a preparation method and application thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the present invention provides a thermal barrier coating material,chemical composition is (Gd) x Sm y Yb 1-x-y ) 2 (A 1-n B n ) 2 O 7 X + y is less than or equal to 0.6, x is more than or equal to 0.2, y is more than or equal to 0.2, A is Zr or Hf, B is Ce, and n is less than or equal to 0.5.
Preferably, y =0.3 to 0.4, n =0 to 0.3.
The invention provides a preparation method of the thermal barrier coating material in the technical scheme, which comprises the following steps:
respectively carrying out first calcination on the metal oxide raw materials corresponding to the thermal barrier coating material to obtain corresponding metal oxide powder;
and mixing and ball-milling the corresponding metal oxide powder, and then carrying out secondary calcination to obtain the thermal barrier coating material.
Preferably, the temperature of the first calcination is 600-1200 ℃, and the time is more than or equal to 2h; the temperature of the second calcination is 1450-1650 ℃, and the time is more than or equal to 6h.
The invention provides a preparation method of the thermal barrier coating material in the technical scheme, which comprises the following steps:
mixing the metal salt mixed solution corresponding to the thermal barrier coating material with ammonia water, and performing coprecipitation to obtain a precursor precipitate;
and sequentially carrying out first calcination and second calcination on the precursor precipitate to obtain the thermal barrier coating material.
Preferably, the temperature of the first calcination is 1300 ℃ and the time is 12 hours, and the temperature of the second calcination is more than or equal to 1400 ℃ and the time is 24 hours.
The invention provides a preparation method of the thermal barrier coating material in the technical scheme, which comprises the following steps:
mixing the metal salt mixed solution corresponding to the thermal barrier coating material with an organic decoction agent, and sequentially carrying out sol and gelation to obtain gel;
and sequentially carrying out first calcination and second calcination on the gel to obtain the thermal barrier coating material.
Preferably, the organic decocting agent is citric acid, polyethylene glycol, ammonium citrate, polyvinylpyrrolidone or EDTA; the temperature of the sol is room temperature, and the time is 6-12 h; the temperature of the gelatinization is 85-100 ℃; the temperature of the first calcination is 1300 ℃, the time is more than or equal to 6h, and the temperature of the second calcination is 1400 ℃, the time is more than or equal to 6h.
The invention provides the application of the thermal barrier coating material in the technical scheme or the thermal barrier coating material prepared by the preparation method in the technical scheme in a high-temperature hot end component of an aeroengine or a gas turbine; the surface temperature of the high-temperature hot end component is 1400-1600 ℃.
The invention provides a thermal barrier coating with a double-ceramic-layer structure, which comprises an alloy substrate layer, a metal bonding layer and a double-ceramic thermal barrier layer which are sequentially stacked; the dual ceramic thermal barrier layer comprises a YSZ bottom layer and a thermal barrier ceramic top layer; the thermal barrier ceramic top layer is the thermal barrier coating material in the technical scheme or the thermal barrier coating material prepared by the preparation method in the technical scheme.
The invention provides a thermal barrier coating material, which takes a rare earth zirconate crystal structure as a target, fully considers the requirements of infrared radiation, high thermal expansion coefficient, low thermal conductivity and high fracture toughness of overtemperature service and passes through Gd 3+ 、Sm 3+ And Yb 3+ Reconstructing pyrochlore crystal structure by using ternary rare earth, regulating and controlling optimized component proportion, increasing crystal defect concentration and adopting Yb 3+ The substitution of the material enhances the lattice distortion, effectively reduces the high-temperature infrared radiation heat transfer, and on the basis of ensuring the low thermal conductivity and high thermal expansion coefficient of the material, high fracture toughness and excellent high temperature resistance are realized, and the service life of the coating is further prolonged. Further, the present invention is achieved by Ce 4+ For part of Zr 4+ Or Hf 4+ The substitution of crystal lattice positions can further increase the defect concentration of the whole crystal, further reduce the thermal conductivity of the material and improve the performances of corrosion resistance, high temperature resistance, fracture toughness and the like. Therefore, the ultrahigh-temperature thermal barrier ceramic material provided by the invention has good high-temperature sintering resistance and phase stability, does not change phase at room temperature to 1600 ℃, and the change rate of the sintering diffusivity of the prepared thermal barrier ceramic coating within the range of 1000-1500 ℃ for 100h is less than or equal to 25%.
The invention provides a preparation method of the thermal barrier coating material, which is synthesized by adopting a solid-phase reaction method, a coprecipitation method or a sol-gel method, forms the thermal barrier coating by atmospheric plasma spraying, is used for high-temperature hot end parts of an aeroengine or a gas turbine, and has the highest service temperature of 1400-1600 ℃ and long thermal shock resistance cycle life.
The thermal conductivity of the thermal barrier coating (conventional laminated structure) with a double-ceramic-layer structure prepared by the thermal barrier coating material is less than or equal to 1.2W/m.K, and the fracture toughness of a sintered ceramic block is more than or equal to 2.1 MPa.m 1/2 And the fracture toughness is obviously improved.
The thermal barrier coating with the double-ceramic-layer structure prepared by the invention has the advantages that YSZ is arranged at the bottom layer, the thermal barrier coating material is positioned at the top layer, the total thickness of the double-ceramic-layer structure can reach 600-1500 mu m, the isothermal thermal cycle life (24 h daily cycle) of the whole thermal barrier coating system at 1100 ℃ is more than or equal to 50 times, and the thermal cycle life is more than or equal to 12000 times in a gas flame thermal gradient cycle test.
Drawings
FIG. 1 is (Sm) prepared in example 1 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 XRD pattern of the powder;
FIG. 2 is (Sm) for plasma spraying prepared in example 1 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 SEM image of the cross section of the powder;
FIG. 3 is a cross-sectional SEM image of a dual ceramic layer high temperature thermal barrier coating prepared by application example 1;
FIG. 4 is a SEM image of a cross section of a dual-ceramic-layer high-temperature thermal barrier coating prepared in application example 2.
Detailed Description
The invention provides a thermal barrier coating material, the chemical composition of which is (Gd) x Sm y Yb 1-x-y ) 2 (A 1-n B n ) 2 O 7 X + y is less than or equal to 0.6, x is more than or equal to 0.2, y is more than or equal to 0.2, A is Zr or Hf, B is Ce, and n is less than or equal to 0.5.
In the present invention, y =0.3 to 0.4, n =0 to 0.3; the thermal barrier coating material is specifically (Sm) 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 、(Sm 0.4 Gd 0.2 Yb 0.4 ) 2 (Hf 0.7 Ce 0.3 ) 2 O 7 、(Sm 0.3 Gd 0.2 Yb 0.5 ) 2 (Zr 0.7 Ce 0.3 ) 2 O 7 Or (Sm) 0.2 Gd 0.4 Yb 0.4 ) 2 Hf 2 O 7 。
The invention provides a preparation method of the thermal barrier coating material in the technical scheme, which comprises the following steps:
respectively carrying out first calcination on the metal oxide raw materials corresponding to the thermal barrier coating material to obtain corresponding metal oxide powder;
and mixing and ball-milling the corresponding metal oxide powder, and then carrying out secondary calcination to obtain the thermal barrier coating material.
In the present invention, unless otherwise specified, all the starting materials required for the preparation are commercially available products well known to those skilled in the art.
The method comprises the steps of respectively carrying out first calcination on metal oxide raw materials corresponding to the thermal barrier coating material to obtain corresponding metal oxide powder.
In the invention, the raw material of the metal oxide corresponding to the thermal barrier coating material is preferably monoclinic phase ZrO 2 (purity is more than or equal to 99.9 percent) and HfO 2 (purity is more than or equal to 99.9 percent) CeO 2 (purity is more than or equal to 99.99 percent) and Gd 2 O 3 (purity is more than or equal to 99.99 percent) and Sm 2 O 3 (purity is more than or equal to 99.99%) and Yb 2 O 3 (the purity is more than or equal to 99.99%).
In the present invention, the first calcination is preferably carried out in an air atmosphere, and the temperature of the first calcination is preferably 600 to 1200 ℃, and the time is preferably not less than 2 hours, and more preferably 4 hours. According to the invention, adsorbed water vapor and other volatile substances are removed through the first calcination, so that the accuracy of the stoichiometric ratio during raw material weighing is ensured.
After the first calcination is completed, the product obtained is preferably cooled to 120 ℃ along with the furnace and transferred to a vacuum drying oven for storage and standby.
After the corresponding metal oxide powder is obtained, the corresponding metal oxide powder is mixed and ball-milled, and then the second calcination is carried out, so as to obtain the thermal barrier coating material.
In the invention, the mixing ball milling mode is preferably wet ball milling, the mixing ball milling preferably adopts zirconia balls as a ball milling medium, water or absolute ethyl alcohol as a liquid medium, and the particle size of powder particles obtained after ball milling is preferably less than or equal to 5 μm. The invention has no special limit on the dosage of the liquid medium and the ball milling medium, and can be adjusted according to the actual requirement. The specific parameters of the mixing ball mill are not specially limited, and the powder particles with the required particle size can be obtained by adjusting according to actual requirements. In the embodiment of the invention, the rotation speed of the ball mill is 240r/min, and the time is 72h.
After the mixing and ball milling are completed, the obtained slurry is preferably transferred to an oven for drying, the obtained dried cake is crushed and sieved by a 300-mesh sieve, and mixed powder is obtained. In the invention, the drying temperature is preferably 120 ℃, and the drying time is preferably 48 hours; the crushing mode is preferably mechanical grinding crushing, and the specific process of the mechanical grinding crushing is not particularly limited in the invention and can be carried out according to the process well known in the art.
After the mixed powder is obtained, the mixed powder is preferably subjected to secondary calcination to obtain the thermal barrier coating material. In the invention, the temperature of the second calcination is preferably 1450-1650 ℃, more preferably 1550 ℃, and the time is preferably more than or equal to 6 hours, more preferably 24 hours; the second calcination is preferably carried out in a high temperature box-type resistance furnace.
After the second calcination is completed, the obtained product is preferably cooled to room temperature along with the furnace, and the thermal barrier coating material is obtained after mechanical crushing; the present invention is preferably mechanically crushed to an average particle size of 5 μm or less, more preferably 1 μm.
The invention provides a preparation method of the thermal barrier coating material in the technical scheme, which comprises the following steps:
mixing the metal salt mixed solution corresponding to the thermal barrier coating material with ammonia water, and performing coprecipitation to obtain a precursor precipitate;
and sequentially carrying out first calcination and second calcination on the precursor precipitate to obtain the thermal barrier coating material.
The invention mixes the metal salt mixed solution corresponding to the thermal barrier coating material with ammonia water, and performs coprecipitation to obtain a precursor precipitate.
In the invention, the preparation process of the metal salt mixed solution corresponding to the thermal barrier coating material is preferably to mix Sm according to a stoichiometric ratio 2 O 3 (purity 99.99%) and Gd 2 O 3 (purity 99.99%) Yb 2 O 3 (purity 99.99%) and CeO 2 (purity 99.99%) are respectively dissolved in fuming nitric acid, and water produced in the dissolving process and unreacted residual nitric acid are fully evaporated to obtain four kinds of rare earth nitrate transparent crystals; respectively adding water into the four rare earth nitrate transparent crystals to prepare four nitrate solutions with the concentration of 1 mol/L; mixing and stirring the four nitrates for 120min, and adding HfOCl according to the stoichiometric ratio 2 ·8H 2 O powder (or ZrOCl 2 ·8H 2 And O) adding the mixture into the mixed solution, and uniformly stirring to obtain a metal salt mixed solution corresponding to the thermal barrier coating material. The stirring rate is not particularly limited in the present invention, and the materials are uniformly mixed according to a process well known in the art.
In the invention, the process of mixing the metal salt mixed solution corresponding to the thermal barrier coating material with ammonia water is preferably to drop ammonia water into the metal salt mixed solution corresponding to the thermal barrier coating material until the pH =12.5 of the solution and no new precipitate appears, and stop dropping ammonia water, wherein the concentration of ammonia water is preferably 15wt%.
After the ammonia water is dripped, the obtained product is preferably continuously stirred for more than or equal to 60min and aged for 120min, and the obtained product is sequentially centrifuged, filtered, dried and crushed and is sieved by more than or equal to 120 meshes to obtain a precursor precipitate.
In the invention, the drying temperature is preferably 120 ℃, and the drying time is preferably 36h; the present invention is not particularly limited with respect to the specific procedures of centrifugation, filtration and disruption, and may be carried out according to procedures well known in the art.
After the precursor precipitate is obtained, the precursor precipitate is sequentially subjected to first calcination and second calcination to obtain the thermal barrier coating material.
In the present invention, the temperature of the first calcination is preferably 1300 ℃ and the time is preferably 12 hours.
After the first calcination is completed, the obtained material is preferably crushed, sieved by a 120-mesh sieve and subjected to second calcination; the temperature of the second calcination is preferably more than or equal to 1400 ℃, and the time is preferably 24h.
After the second calcination is completed, the obtained material is preferably cooled to room temperature, and is ground and crushed to 60 nm-2 μm to obtain the thermal barrier coating material. The process of grinding and crushing is not particularly limited, and the material with the particle size requirement can be obtained. Both the first calcination and the second calcination are preferably carried out in a high temperature box-type resistance furnace.
The invention provides a preparation method of the thermal barrier coating material in the technical scheme, which comprises the following steps:
mixing the metal salt mixed solution corresponding to the thermal barrier coating material with an organic decoction agent, and sequentially carrying out sol and gelation to obtain gel;
and sequentially carrying out first calcination and second calcination on the gel to obtain the thermal barrier coating material.
According to the invention, a metal salt mixed solution corresponding to the thermal barrier coating material is mixed with an organic decoction agent, and sol and gelation are sequentially carried out to obtain gel.
In the invention, the preparation process of the metal salt mixed solution corresponding to the thermal barrier coating material preferably comprises the step of mixing Sm according to a stoichiometric ratio 2 O 3 (purity 99.99%) and Gd 2 O 3 (purity 99.99%) Yb 2 O 3 (purity 99.99%) CeO 2 (purity 99.99%) were dissolved in fuming nitric acid, respectively, and H produced in the dissolving process was dissolved 2 Fully evaporating the O and the unreacted residual nitric acid to obtain four rare earth nitrate crystals, and respectively adding water into the four rare earth nitrate crystals to prepare four nitrate solutions with the concentration of 1 mol/L; mixing the four nitrate solutions, stirring for 60min, and adding AOCl according to stoichiometric ratio 2 ·8H 2 O or A (NO) 3 ) 4 ·6H 2 Adding O powder into the mixed solution, and stirring uniformly. The stirring rate is not particularly limited in the present invention, and the materials are uniformly mixed according to a process well known in the art.
In the invention, the organic decocting agent is preferably citric acid, polyethylene glycol, ammonium citrate, polyvinylpyrrolidone or EDTA; the molar ratio of the organic sequestering agent to the total molar amount of all metal ions in the metal salt mixed solution is preferably 1.2. The process of mixing the metal salt mixed solution corresponding to the thermal barrier coating material and the organic chelating agent is not particularly limited, and the process can be carried out according to the process known in the art.
In the invention, the temperature of the sol is preferably room temperature, and the time is preferably 6-12 h; the solvolysis is preferably carried out under stirring.
After the sol is finished, the mixed molten salt is preferably placed in a constant-temperature water bath kettle for gelation; the temperature of the gelation is preferably 85 to 100 ℃; in the present invention, the time for the gelation is not particularly limited, and the water content may be sufficiently evaporated. According to the invention, water is evaporated through a constant-temperature water bath kettle, and the solution is gradually converted into sol. After the gelation is completed, the present invention preferably grinds and crushes the resultant material to obtain a dried gel. The process of the present invention for grinding and crushing is not particularly limited, and may be performed according to a process well known in the art.
After the gel is obtained, the gel is sequentially subjected to first calcination and second calcination to obtain the thermal barrier coating material.
In the present invention, the first calcination and the second calcination are preferably performed in a high-temperature box-type resistance furnace; the temperature of the first calcination is preferably 1300 ℃, and the time is preferably more than or equal to 6h.
After the first calcination is completed, the obtained material is preferably crushed and then subjected to second calcination; the temperature of the second calcination is preferably 1400 ℃, and the time is preferably more than or equal to 6h.
After the second calcination is completed, the present invention preferably crushes the obtained material to obtain the thermal barrier coating material with the desired particle size, preferably 60nm to 1 μm, more preferably 80 to 300nm.
The invention provides the application of the thermal barrier coating material in the technical scheme or the thermal barrier coating material prepared by the preparation method in the technical scheme in a high-temperature hot end component of an aeroengine or a gas turbine; the surface temperature of the high-temperature hot end component is 1400-1600 ℃. In the present invention, the high-temperature hot-end component is preferably a combustor inner wall, a turbine moving blade, a turbine stationary blade, or a nozzle.
The invention provides a thermal barrier coating with a double-ceramic-layer structure, which comprises an alloy substrate layer, a metal bonding layer and a double-ceramic thermal barrier layer which are sequentially stacked; the dual ceramic thermal barrier layer comprises a YSZ bottom layer and a thermal barrier ceramic top layer; the thermal barrier ceramic top layer is the thermal barrier coating material in the technical scheme or the thermal barrier coating material prepared by the preparation method in the technical scheme.
In the present invention, the alloy substrate layer is preferably a nickel-based superalloy, more preferably a cast superalloy or a directionally solidified superalloy or a single crystal superalloy; the specific grade and size of the nickel-based superalloy are not particularly limited in the invention, and any commercially available grade well known in the art can be used; in the embodiment of the invention, the alloy is specifically a directional solidification nickel-base superalloy DZ125, a directional solidification superalloy MAR247 or a GH3128/3230 superalloy or a nickel-base single crystal superalloy DD10, and the sizes of the alloy are phi 30mm multiplied by 5mm round pieces.
In the present invention, the nickel-base superalloy is preferably pretreated before use; the pretreatment process is preferably that the nickel-based superalloy substrate is subjected to sand blasting treatment on one surface of a wafer by using 60-mesh corundum under 0.4MPa compressed air until the surface roughness Ra =3 mu m, then ultrasonic cleaning is carried out by using acetone, and drying is carried out in an oven at 120 ℃.
In the invention, the composition of the metal bonding layer preferably comprises NiCoCrAlY, and preferably also comprises less than or equal to 2wt.% of one or more of Hf, ta and Si elements; the thickness of the metal adhesive layer is preferably 100 to 200 μm, and more preferably 120 to 150 μm. The specific composition and content of the metal bonding layer are not particularly limited in the present invention, and any commercially available product well known in the art may be used.
The invention preferably adopts supersonic flame spraying (HVOF/HVAF) or low-pressure plasma spraying (LPPS) to prepare a metal bonding layer on the alloy substrate; the present invention does not specifically limit the specific process and parameters for preparing the metal bonding layer, and the process is performed according to the process known in the art.
In the invention, the dual ceramic thermal barrier layer comprises a YSZ bottom layer and a thermal barrier ceramic top layer; the YSZ bottom layer is preferably yttrium oxide (Y) 2 O 3 3-5% mol fraction) of partially stabilized zirconia (YSZ); the thickness of the YSZ bottom layer is preferably 60-300 μm, and more preferably 100-200 μm; the porosity is preferably 5 to 12%, more preferably 8 to 10%.
The invention preferably adopts the atmospheric plasma spraying to prepare the YSZ bottom layer on the surface of the metal bonding layer; the specific process and parameters of the atmospheric plasma spraying are not particularly limited in the present invention, and may be performed according to the processes well known in the art.
In the invention, the thermal barrier ceramic top layer is the thermal barrier coating material in the technical scheme or the thermal barrier coating material prepared by the preparation method in the technical scheme, and the thermal barrier ceramic top layer is preferably prepared on the surface of the YSZ bottom layer by adopting atmospheric plasma spraying; the specific process and parameters of the atmospheric plasma spraying are not particularly limited in the present invention, and may be performed according to the processes well known in the art.
The thermal barrier coating material is preferably agglomerated into powder with the particle size of 20-150 mu m by adopting a spray granulation method, and the powder is directly used for preparing the thermal barrier coating by atmospheric plasma spraying; or the agglomerated powder is preferably further sintered or spheroidized by plasma and then used for preparing the thermal barrier coating by atmospheric plasma spraying. The sintering and plasma spheroidizing process is not particularly limited in the present invention, and may be performed according to a process well known in the art. In an application example of the invention, the sintering is carried out for 12 hours at 800 ℃.
In the present invention, the thickness of the thermal barrier ceramic top layer is preferably 400 to 1450 μm, more preferably 500 to 800 μm.
In the present invention, the total thickness of the double ceramic thermal barrier layers is preferably 600 to 1500 μm.
In the invention, the structure of the thermal barrier ceramic top layer is preferably a classic layered porous structure, the porosity is preferably 10-30%, more preferably 20%, and the thermal conductivity in a spraying state is preferably less than or equal to 1.2 W.m -1 ·K -1 (ii) a Alternatively, the structure of the thermal barrier ceramic top layer is preferably a vertical crack structure, the vertical crack density of the vertical crack structure is preferably 1 to 13 strips/mm ((the number of vertical cracks within a width range of 1mm parallel to the interface direction of the coating and the substrate), more preferably 1.8 to 7 strips/mm, and the total porosity of the coating is preferably 6 to 20%, more preferably 10 to 15%, and further preferably 12%.
The vertical crack structure refers to the section of the coating, the general direction is vertical to the interface of the coating and the metal substrate, and the length is more than 1/2 of the total thickness of the coating.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparation of powder (Sm) by high temperature solid phase synthesis 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 ：
Is reacted with ZrO 2 (purity 99.9%) and Sm 2 O 3 (purity 99.99%) and Gd 2 O 3 (purity 99.99%) Yb 2 O 3 (purity 99.99%) calcining the four kinds of powder at 600 ℃ for 4h, weighing the four kinds of powder according to stoichiometric ratio, putting the powder into a ball milling tank, adding zirconia ball milling balls into the ball milling tank, adding deionized water, ball milling and mixing for 72h, wherein the rotating speed of the ball milling tank is 240r/min, completely transferring slurry in the ball milling tank into a stainless steel container after ball milling and mixing, drying for 48h at 120 ℃ in an oven, and dryingMechanically grinding and crushing the dried material cake and sieving the material cake with a 300-mesh sieve; placing the sieved mixed powder in a high-temperature box type resistance furnace, keeping the temperature at 1450 ℃ for 24h, cooling the mixed powder to room temperature along with the furnace, and mechanically crushing the mixed powder until the average particle size is less than or equal to 5 mu m to obtain the Sm 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 And (3) powder.
Example 2
Preparing powder (Sm) by adopting coprecipitation way 0.4 Gd 0.2 Yb 0.4 ) 2 (Hf 0.7 Ce 0.3 ) 2 O 7 ：
Weighing Sm according to stoichiometric ratio 2 O 3 (purity 99.99%) and Gd 2 O 3 (purity 99.99%) Yb 2 O 3 (purity 99.99%) CeO 2 (purity 99.99%) were dissolved in fuming nitric acid, respectively, and H produced in the dissolving process was dissolved 2 Fully evaporating the O and the unreacted nitric acid to obtain four rare earth nitrate crystals; respectively adding deionized water into the four rare earth nitrate crystals to prepare four nitrate solutions with the concentration of 1 mol/L; mixing and stirring the four nitrate solutions for 120min, and weighing HfOCl according to the stoichiometric ratio 2 ·8H 2 Adding O powder into the obtained mixed solution, and uniformly stirring; dropwise adding ammonia water with the concentration of 15wt% into the five mixed salt solutions while continuously stirring until the pH =12.5 of the solution and no new precipitate appears, stopping dropwise adding, continuously stirring for 60min, then aging for 120min, centrifuging and filtering the obtained precipitated mixture, and drying for 36h at 120 ℃ in an oven; grinding and crushing the dried material cake, sieving with a 120-mesh sieve, putting the sieved mixed powder into a high-temperature box-type resistance furnace, firstly preserving the heat at 1300 ℃ for 12 hours, taking out the powder, crushing and sieving with the 120-mesh sieve, continuously preserving the heat at 1400 ℃ for 24 hours, cooling the powder to room temperature along with the furnace, grinding and crushing the powder until the particle size is 60 nm-2 mu m to obtain the (Sm) powder 0.4 Gd 0.2 Yb 0.4 ) 2 (Hf 0.7 Ce 0.3 ) 2 O 7 And (3) powder.
Example 3
Preparation of powder (Sm) by the Sol-gel route 0.3 Gd 0.2 Yb 0.5 ) 2 (Zr 0.7 Ce 0.3 ) 2 O 7 ：
Weighing Sm according to stoichiometric ratio 2 O 3 (purity 99.99%) and Gd 2 O 3 (purity 99.99%) Yb 2 O 3 (purity 99.99%) CeO 2 (purity 99.99%) are dissolved in fuming nitric acid respectively, and H produced in the dissolving process is dissolved 2 Evaporating the O and the unreacted nitric acid to obtain four transparent rare earth nitrate crystals; respectively adding deionized water into the four rare earth nitrate transparent crystals to prepare four nitrate solutions with the concentration of 1 mol/L; mixing and stirring the four nitrate solutions for 60min, and weighing an appropriate amount of ZrOCl according to a stoichiometric ratio 2 ·8H 2 Adding O powder into the mixed solution, and dissolving and stirring uniformly;
weighing citric acid (according to the molar ratio of citric acid: all metal ions = 1.2) and adding the citric acid into the four rare earth nitrate aqueous solutions, stirring and mixing at room temperature for 12 hours, and putting the obtained mixed molten salt into a constant-temperature water bath kettle at 85 ℃ until water is fully evaporated to obtain dry gel powder;
grinding and crushing the dried gel powder, placing the gel powder in a high-temperature box type resistance furnace, firstly preserving heat for 6h at 1300 ℃, then taking out the gel powder, grinding and crushing the gel powder, then preserving heat for 6h at 1400 ℃, and grinding and crushing the gel powder to obtain (Sm) with the particle size of 60-300 nm 0.3 Gd 0.2 Yb 0.5 ) 2 (Zr 0.7 Ce 0.3 ) 2 And (3) O powder.
Example 4
Preparation of powder (Sm) by high temperature solid phase synthesis 0.2 Gd 0.4 Yb 0.4 ) 2 Hf 2 O 7 ：
To mix HfO 2 (purity 99.9%) and Sm 2 O 3 (purity 99.99%) and Gd 2 O 3 (purity 99.99%) Yb 2 O 3 (purity 99.99%) four powders were calcined at 1200 ℃ for 2h; weighing four kinds of powder according to a stoichiometric ratio, filling the powder into a ball milling tank, adding zirconia balls into the ball milling tank, adding deionized water, carrying out ball milling and mixing for 72 hours, wherein the rotating speed of the ball milling tank is 240r/min, and completely transferring slurry in the ball milling tank after ball milling and mixing are finishedPlacing into a stainless steel container, drying in an oven at 120 deg.C for 48 hr, mechanically grinding and crushing the dried cake, sieving with 300 mesh sieve, placing the sieved mixed powder in a high temperature box-type resistance furnace, keeping the temperature at 1550 deg.C for 24 hr, cooling to room temperature, and mechanically crushing to obtain (Sm) powder with average particle diameter of 1 μm 0.2 Gd 0.4 Yb 0.4 ) 2 Hf 2 O 7 And (3) powder.
Application example 1
(Sm) prepared in example 1 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 Spray granulating the powder, screening the powder with the particle size of 20-150 mu m, sintering the powder at 800 ℃ for 12h to obtain (Sm) for plasma spraying 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 Powder;
takes directional solidification nickel-based superalloy DZ125 as a matrix with the size of
The wafer is prepared by performing sand blasting treatment on one surface of the wafer by adopting 60-mesh corundum under 0.4MPa of compressed air until the surface roughness Ra =3 mu m, then performing ultrasonic cleaning by using acetone, and drying in a 120 ℃ oven;
preparing a NiCoCrAlYTa metal bonding layer with the thickness of 150 mu m on the surface of a circular DZ125 high-temperature alloy test piece by adopting supersonic speed flame spraying HVOF;
preparing a YSZ (American 204NS series powder) ceramic thermal barrier layer with the thickness of 150 mu m on the metal bonding layer by adopting atmospheric plasma spraying, wherein the porosity is 8%;
preparing a layer of (Sm) with the thickness of 1450 mu m on the surface of the YSZ layer by adopting atmospheric plasma spraying 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 The coating of the thermal barrier ceramic surface layer is in a vertical crack (DVC) structure, the vertical crack density is 1.8 strips/mm, and the total porosity of the coating is 15 percent, so that the double-ceramic-layer high-temperature thermal barrier coating is obtained.
Application example 2
Spray granulation of (Sm) prepared in example 2 0.4 Gd 0.2 Yb 0.4 ) 2 (Hf 0.7 Ce 0.3 ) 2 O 7 Obtaining hollow spherical agglomerated particles with the particle size of 40-90 mu m by powder for preparing the thermal barrier coating;
using single crystal superalloy DD10 as a substrate with a size of
The wafer is prepared by performing sand blasting treatment on one surface of the wafer by adopting 60-mesh corundum under 0.4MPa of compressed air until the surface roughness Ra =3 mu m, then performing ultrasonic cleaning by using acetone, and drying in a 120 ℃ oven;
preparing a NiCoCrAlYHf metal bonding layer with the thickness of 200 mu m on the surface of a nickel-based single crystal superalloy round test piece by adopting a low-pressure plasma spraying method;
preparing a YSZ (American 204NS series powder) ceramic thermal barrier layer with the thickness of 300 mu m on the metal bonding layer by adopting atmospheric plasma spraying, wherein the porosity is 10%;
preparing a layer of (Sm) with the thickness of 550 mu m on the surface of the YSZ layer by adopting atmospheric plasma spraying 0.4 Gd 0.2 Yb 0.4 ) 2 (Hf 0.7 Ce 0.3 ) 2 O 7 The thermal barrier ceramic surface layer is a classical layered porous structure, the porosity of the coating is 20%, and the thermal conductivity in a spraying state is 0.59 W.m -1 ·K -1 And obtaining the double-ceramic-layer high-temperature thermal barrier coating.
Application example 3
(Sm) prepared in example 3 0.3 Gd 0.2 Yb 0.5 ) 2 (Zr 0.7 Ce 0.3 ) 2 After the O powder is subjected to spray granulation, sintering for 12 hours at 1000 ℃ to obtain powder with the particle size of 45-125 mu m for preparing a thermal barrier coating;
GH3128/3230 high-temp alloy as matrix and its size is
The wafer is prepared by performing sand blasting treatment on one surface of the wafer by adopting 60-mesh corundum under 0.4MPa of compressed air until the surface roughness Ra =3 mu m, performing ultrasonic cleaning by using acetone, and drying in a 120 ℃ oven;
preparing a NiCoCrAlY metal bonding layer on the surface of a nickel-based single crystal superalloy round test piece by adopting a low-pressure plasma spraying method, wherein the thickness of the NiCoCrAlY metal bonding layer is 120 mu m;
preparing a layer of YSZ (Y) with the thickness of 60 mu m on the metal bonding layer by adopting atmospheric plasma spraying 2 O 3 Mole fraction 3%) ceramic thermal barrier layer with a porosity of 12%;
preparing a layer of (Sm) with the thickness of 500 mu m on the surface of the YSZ layer by adopting atmospheric plasma spraying 0.3 Gd 0.2 Yb 0.5 ) 2 (Zr 0.7 Ce 0.3 ) 2 O 7 The thermal barrier ceramic surface layer is of a DVC (vertical crack) structure, the vertical crack density is 7cracks/mm, and the porosity of the coating is 12 percent, so that the double-ceramic-layer high-temperature thermal barrier coating is obtained.
Application example 4
(Sm) prepared in example 4 0.2 Gd 0.4 Yb 0.4 ) 2 Hf 2 O 7 Spraying and granulating the powder to form high-fluidity agglomerated powder, and performing plasma spheroidization to obtain powder with the particle size of 20-120 mu m for preparing a thermal barrier coating by atmospheric plasma spraying;
taking directional solidification superalloy MAR247 as a matrix with the size of
The wafer is prepared by carrying out sand blasting treatment on one surface of the wafer by adopting 60-mesh corundum under 0.4MPa of compressed air until the surface roughness Ra =3 mu m, then carrying out ultrasonic cleaning by using acetone, and drying in a 120 ℃ drying oven;
preparing a NiCoCrAlYHfTa metal bonding layer on the surface of the nickel-based single crystal superalloy round test piece by adopting a low-pressure plasma spraying method, wherein the thickness of the NiCoCrAlYHfTa metal bonding layer is 100 mu m;
preparing a layer of YSZ (Y) with the thickness of 200 mu m on the metal bonding layer by adopting atmospheric plasma spraying 2 O 3 Mole fraction 5%) of a ceramic thermal barrier layer with a porosity of 5%;
preparing a layer of (Sm) with the thickness of 800 mu m on the surface of the YSZ layer by adopting atmospheric plasma spraying 0.2 Gd 0.4 Yb 0.4 ) 2 Hf 2 O 7 Thermal barrier ceramic top layer, the top layerThe high-temperature thermal barrier coating with double ceramic layers is obtained by adopting a DVC (vertical crack) structure, wherein the vertical crack density is 13cracks/mm, and the porosity of the coating is 10%.
Characterization and Performance testing
1) FIG. 1 is (Sm) prepared in example 1 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 XRD pattern of the powder; as can be seen from FIG. 1, (Sm) is prepared 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 The powder has high chemical purity reaching 99.9 percent.
2) FIG. 2 is (Sm) for plasma spraying prepared in example 1 0.2 Gd 0.2 Yb 0.6 ) 2 Zr 2 O 7 As is clear from fig. 2, the cross-sectional SEM image of the powder shows that the agglomerate has a certain porosity, but the density of the single-particle agglomerate is significantly higher than that in the spray granulation. The powder particle morphology has an important influence on the porosity of the plasma spraying coating, the growth and the density of vertical cracks.
3) Fig. 3 is a cross-sectional SEM image of the dual-ceramic-layer high-temperature thermal barrier coating prepared in application example 1, and the dual-layer structure of the YSZ bottom layer and the thermal barrier ceramic material surface layer can be clearly seen.
4) Fig. 4 is a SEM image of a cross-section of a dual-ceramic-layer high-temperature thermal barrier coating prepared in application example 2, and a dual-layer structure of a YSZ bottom layer and a thermal barrier ceramic material surface layer can be clearly seen.
5) The results of laser thermal conductivity tests on the double-ceramic-layer high-temperature thermal barrier coatings prepared in the application examples 1 to 4 show that the average thermal conductivity of the thermal barrier coatings prepared in the application examples 1 to 4 in a spraying state is 1.20Wm -1 K -1 、0.54Wm -1 K -1 、1.16Wm -1 K -1 And 0.86Wm -1 K -1 (ii) a The sintering diffusivity change rates of the sprayed coating within the range of 1000-1500 ℃ for 100h are respectively as follows: 22%, 25%, 20% and 18%.
6) The fracture toughness test of the double-ceramic-layer high-temperature thermal barrier coatings prepared in the examples 1 to 4 is carried out by a unilateral incision method, and the test results are respectively as follows: 3.2 MPa.m 1/2 、2.8MPa·m 1/2 、3.8MPa·m 1/2 And 3.5 MPa.m 1/2 。
7) The double-ceramic-layer high-temperature thermal barrier coatings prepared in the application examples 1-4 are subjected to isothermal thermal cycle life test, and the test method comprises the following steps: placing the sample in an electric furnace, keeping the temperature at 1100 ℃ for 23.5h, taking the sample out of the electric furnace, placing the sample in room-temperature air for cooling for 30min, and recording as one thermal cycle and daily cycle; the results show that the isothermal thermal cycle life (24 h day cycle) of the thermal barrier coatings prepared in the application examples 1 to 4 are as follows: not less than 120 times, not less than 65 times, not less than 115 times and not less than 150 times.
8) Carrying out a gas flame thermal gradient cycle test on the double-ceramic-layer high-temperature thermal barrier coatings prepared in the examples 1-4, wherein the test temperature of the surface of the coating is 1400-1600 ℃, heating the surface of the coating for 5min by flame, then removing the flame, and cooling for 2min;
the result shows that the thermal shock resistance cycle life of the gas flame of the high-temperature thermal barrier coating with the double ceramic layers prepared in the application example 1 reaches 28000 times at the surface test temperature of 1500 ℃.
The service temperature of the double-ceramic-layer high-temperature thermal barrier coating prepared in application example 2 is 1600 ℃, and the thermal shock resistance cycle life of gas flame is 23000 times as long as the maximum.
The application example 3 is that the use temperature of the double-ceramic-layer high-temperature thermal barrier coating is not more than 1600 ℃, and the thermal shock resistance cycle life of the gas flame is 25000 times as long.
The application example 4 is that the service temperature of the double-ceramic-layer high-temperature thermal barrier coating is 1600 ℃, and the thermal shock resistance cycle life of gas flame is up to 30000 times.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A thermal barrier coating material is characterized in that the chemical composition is (Gd) x Sm y Yb 1-x-y ) 2 (A 1-n B n ) 2 O 7 X + y is less than or equal to 0.6, x is more than or equal to 0.2, y is more than or equal to 0.2, A is Zr or Hf, B is Ce, and n is less than or equal to 0.5.
2. The thermal barrier coating material of claim 1, wherein y = 0.3-0.4, n = 0-0.3.
3. A method for producing a thermal barrier coating material as claimed in claim 1 or 2, characterized in that it comprises the following steps:
respectively carrying out first calcination on the metal oxide raw materials corresponding to the thermal barrier coating material to obtain corresponding metal oxide powder;
and mixing and ball-milling the corresponding metal oxide powder, and then carrying out secondary calcination to obtain the thermal barrier coating material.
4. The preparation method according to claim 3, characterized in that the temperature of the first calcination is 600-1200 ℃ and the time is not less than 2h; the temperature of the second calcination is 1450-1650 ℃, and the time is more than or equal to 6h.
5. Method for the production of a thermal barrier coating material according to claim 1 or 2, characterized in that it comprises the following steps:
mixing the metal salt mixed solution corresponding to the thermal barrier coating material with ammonia water, and performing coprecipitation to obtain a precursor precipitate;
and sequentially carrying out first calcination and second calcination on the precursor precipitate to obtain the thermal barrier coating material.
6. The preparation method according to claim 5, characterized in that the temperature of the first calcination is 1300 ℃ and the time is 12h, and the temperature of the second calcination is more than or equal to 1400 ℃ and the time is 24h.
7. A method for producing a thermal barrier coating material as claimed in claim 1 or 2, characterized in that it comprises the following steps:
mixing the metal salt mixed solution corresponding to the thermal barrier coating material with an organic decoction agent, and sequentially carrying out sol and gelation to obtain gel;
and sequentially carrying out first calcination and second calcination on the gel to obtain the thermal barrier coating material.
8. The method of claim 7, wherein the organic chelating agent is citric acid, polyethylene glycol, ammonium citrate, polyvinylpyrrolidone or EDTA; the temperature of the sol is room temperature, and the time is 6-12 h; the temperature of the gelatinization is 85-100 ℃; the temperature of the first calcination is 1300 ℃, the time is more than or equal to 6h, and the temperature of the second calcination is 1400 ℃, the time is more than or equal to 6h.
9. Use of the thermal barrier coating material of claim 1 or 2 or the thermal barrier coating material prepared by the preparation method of any one of claims 3 to 8 in a high-temperature hot-end component of an aeroengine or a gas turbine; the surface temperature of the high-temperature hot end component is 1400-1600 ℃.
10. A thermal barrier coating with a double-ceramic-layer structure is characterized by comprising an alloy substrate layer, a metal bonding layer and a double-ceramic thermal barrier layer which are sequentially stacked; the dual ceramic thermal barrier layer comprises a YSZ bottom layer and a thermal barrier ceramic top layer; the thermal barrier ceramic top layer is the thermal barrier coating material described in claim 1 or 2 or the thermal barrier coating material prepared by the preparation method described in any one of claims 3 to 8.
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