CN118326309A - Preparation method of nano-structure high-entropy cerium zirconate sprayable powder and ultra-high temperature thermal barrier coating - Google Patents
Preparation method of nano-structure high-entropy cerium zirconate sprayable powder and ultra-high temperature thermal barrier coating Download PDFInfo
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T50/00—Aeronautics or air transport
- Y02T50/60—Efficient propulsion technologies, e.g. for aircraft
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- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a nano-structure high-entropy cerium zirconate spray powder material and a preparation method of an ultra-high temperature thermal barrier coating, wherein the spray powder material is A 2B2O7 -10 kinds of zirconate, A consists of 5-10 kinds of elements in La, nd, sm, gd, yb, eu, tb, dy, lu, Y, tm, and B consists of Zr and Ce. The invention has simple equipment and simple and controllable process, the prepared high-entropy powder has a nano structure, high purity, good nano structure retention and fine nano crystal; the prepared ultra-temperature thermal barrier nano coating has a multi-mode structure, excellent fracture toughness, fine grains and good high-temperature phase stability, can improve the high-temperature stability of the existing REZ TBCs, improves the fracture toughness and the thermal expansion coefficient of the REZ TBCs, and can be used as a high-performance nano-structure thermal barrier coating material of an aeroengine and a gas turbine.
Description
Technical Field
The invention belongs to the field of high-temperature thermal protection coatings, and relates to a preparation method of a nano-structure high-entropy cerium zirconate sprayable powder and an ultra-high-temperature thermal barrier coating.
Background
The ceramic coating represented by the Thermal Barrier Coating (TBC) is widely applied to hot end components of aeroengines and gas turbines, protects a high-temperature alloy matrix, plays roles in resisting high temperature, oxidization and abrasion, and has extremely important significance for national defense and national economy construction. The traditional thermal barrier coating surface material is Yttria Stabilized Zirconia (YSZ), the service temperature is lower than 1200 ℃, when the working temperature is higher than 1200 ℃ for a long time, the YSZ can be subjected to phase change and sintering, so that the mechanical property and the thermophysical property of the thermal barrier coating are rapidly deteriorated, the coating is invalid, and the service life of the thermal barrier coating is greatly limited. Second, the higher thermal conductivity of currently used YSZ at 1000 ℃ is about 2.3W/(m·k) and does not provide a large insulating temperature gradient for effective thermal protection of aeroengines and gas turbines. As new generation engines advance to higher thrust weight ratios and longer service times, conventional zirconia-based materials have failed to meet the needs. In recent years, various new thermal barrier coating materials have been developed in place of YSZ, such as Rare Earth Zirconates (REZ), rare Earth Aluminates (REA), rare Earth Tantalates (RET), and the like, having pyrochlore or fluorite structures. The rare earth zirconate has excellent high-temperature stability and lower heat conductivity, but has the main defects of poor fracture toughness, low thermal expansion coefficient and the like, so that the application of the rare earth zirconate in a high-temperature environment is limited.
In recent years, the multicomponent entropy control engineering provides a new approach for the design of thermal barrier coating materials. It is reported that the multi-component high-entropy design enables the high-entropy ceramic to have high entropy effect, lattice distortion effect, cocktail effect and delayed diffusion effect, so that the high-entropy ceramic has relatively higher phase stability, lower heat conductivity, performance adjustability and better high-temperature mechanical property, and the defects of the single-component REZ TBCs material can be overcome. Studies have shown that for a 2B2O7 type zirconate, the a-site high entropy design helps to improve the fracture toughness and thermal expansion coefficient of the REZ, and the B-site high entropy design helps to improve the high temperature phase stability and thermal expansion coefficient of the REZ. However, researches are focused on the ceramic materials per se, and no report on the use of the ceramic materials for thermal spraying of high-entropy powder exists. In addition, with the development of nanotechnology, nano ceramic powders are becoming accepted by researchers because of the positive impact of nanostructured powders on the lifetime of thermally sprayed nanostructured TBCs compared to conventional powders.
Disclosure of Invention
Aiming at the problems of poor high-temperature stability, easy phase change, reduced toughness, unmatched thermal expansion and finally ineffective coating existing in the existing thermal barrier coating, the invention provides a nano-structure high-entropy cerium zirconate sprayable powder and a preparation method of an ultrahigh-temperature thermal barrier coating by carrying out high-entropy design on the A position and doping modification on the B position of A 2B2O7 type zirconate from the material design perspective. The invention has simple equipment and simple and controllable process, the prepared high-entropy powder has a nano structure, high purity, good nano structure retention and fine nano crystal; the prepared ultra-temperature thermal barrier nano coating has a multi-mode structure, excellent fracture toughness, fine grains and good high-temperature phase stability, can improve the high-temperature stability of the existing REZ TBCs, improves the fracture toughness and the thermal expansion coefficient of the REZ TBCs, and can be used as a high-performance nano-structure thermal barrier coating material of an aeroengine and a gas turbine.
The invention aims at realizing the following technical scheme:
The nano-structure high-entropy cerium zirconate spray powder material is A 2B2O7 -10 kinds of element in La, nd, sm, gd, yb, eu, tb, dy, lu, Y, tm; b consists of Zr and Ce, and the stoichiometric ratio of Zr to Ce can be 1: 9. 2: 8. 2.5:7.5, 5: 5. 7.5:2.5, 8: 2. 9:1, etc., as long as the ratio of the sum of the B-site elements and the ratio of the sum of the a-site elements are the same.
The preparation method of the nano-structured high-entropy cerium zirconate spray powder material comprises the following steps:
Step one, weighing nano A 2O3 powder raw materials and nano B 2O3 powder raw materials according to a stoichiometric ratio shown in a chemical formula A 2B2O7, wherein:
The A 2O3 powder raw materials are 5-10 of nano La 2O3 powder, nano Nd 2O3 powder, nano Sm 2O3 powder, nano Gd 2O3 powder, nano Yb 2O3 powder, nano Eu 2O3 powder, nano Tb 2O3 powder, nano Dy 2O3 powder, nano Lu 2O3 powder, nano Y 2O3 powder and nano Tm 2O3 powder;
the nano B 2O3 powder raw materials are nano CeO 2 powder and nano ZrO 2 powder;
The particle sizes of the nano La 2O3 powder, the nano Nd 2O3 powder, the nano Sm 2O3 powder, the nano Gd 2O3 powder, the nano Yb 2O3 powder, the nano Eu 2O3 powder, the nano Tb 2O3 powder, the nano Dy 2O3 powder, the nano Lu 2O3 powder, the nano Y 2O3 powder, the nano Tm 2O3 powder, the nano CeO 2 powder and the nano ZrO 2 powder are all 10-80 nm;
the nano powder raw material has 4N-level purity;
Adding deionized water into a ball mill, adding a dispersing agent into the deionized water, adding the nano powder raw material in the first step after the dispersing agent is completely dissolved, performing ball milling, adding a binder to obtain uniform slurry, and performing spray granulation and solid-phase sintering to obtain nano-structure high-entropy cerium zirconate spherical powder, wherein:
the dosage of the deionized water is 0.5 to 2 times of the total mass of the used nano powder raw materials;
The dispersing agent is one or more of sodium tripolyphosphate (Na 5P3O10), sodium hexametaphosphate ((NaPO 3)6), ammonium citrate (C 6H5O7(NH4)3), sodium citrate (C 6H5Na3O7) and the like, and the dosage of the dispersing agent is 0.05-5% of the total mass of the nano powder raw material;
the diameter of the zirconia grinding ball is 3-8 mm, the mass of the zirconia grinding ball is 1-3 times of the total mass of the nano powder raw material, the ball milling time is 4-12 h, and the revolution is 400-1000 rpm;
The adhesive is one of gum arabic (Acacia), polyvinyl alcohol (PVA), carboxymethyl cellulose (CMC), epoxy resin and the like, and the adhesive is 0.05-10% of the total mass of the nano powder raw material;
the solid phase sintering is carried out in an atmospheric environment, and the conditions of the solid phase sintering are as follows: heating to 1100-1600 ℃ at a speed of 1-15 ℃/min, and preserving heat for 0.5-3 h;
the nano-structure high-entropy cerium zirconate spherical powder is a high-entropy phase with the grain size smaller than 100nm, and the grain size is preferably 20-80 mu m.
The ultra-high temperature thermal barrier coating of a single ceramic layer coating system takes a high temperature alloy as a matrix, an alloy bonding layer and a nano-structure high-entropy cerium zirconate ceramic coating are sequentially arranged on the surface of the matrix, the nano-structure high-entropy cerium zirconate ceramic coating is prepared by spraying a nano-structure high-entropy cerium zirconate sprayable powder material, wherein:
The superalloy substrate can be one or more of nickel-based, cobalt-based, iron-based and other alloys;
the alloy tie layer may be one or more of NiCrAlY, coCrAlY, niCoCrAlY, niCrAlYCe, coCrAlYCe, niCoCrAlYCe;
The thickness of the alloy bonding layer is 80-200 mu m;
the nano-structure high-entropy cerium zirconate ceramic layer is a high-entropy phase and has a thickness of 30-250 mu m.
The preparation method of the ultra-high temperature thermal barrier coating of the single ceramic layer coating system comprises the following steps:
Step one, carrying out grinding, polishing and finishing on the surface of a high-temperature alloy matrix, then carrying out sand blasting treatment to ensure that the surface has certain roughness, then carrying out ultrasonic cleaning on the high-temperature alloy matrix by using ethanol, and then preparing an alloy bonding layer (MCrAlY) on the surface by adopting a thermal spraying technology, wherein:
the thermal spray technique may be one of Atmospheric Plasma Spraying (APS), low Pressure Plasma Spraying (LPPS), supersonic flame spraying (HVOF);
The parameters of the atmospheric plasma spraying are as follows: the spraying distance is 100-300 mm, the powder feeding speed is 5-40 g/min, the carrier gas flow is 6-15 SCFH, the spraying current is 450-600A, the spraying voltage is 45-60V, the main air flow is 30-70 SCFH, and the auxiliary air flow is 5-20 SCFH;
Depositing nano-structure high-entropy cerium zirconate spherical powder on the surface of the alloy bonding layer obtained in the first step by using an APS technology to form a nano-structure high-entropy cerium zirconate ceramic coating, wherein:
the parameters in the preparation process of the nano-structured high-entropy cerium zirconate ceramic coating are as follows: the spraying distance is 50-250 mm, the powder feeding speed is 5-20 g/min, the carrier gas flow is 8-145 CFH, the spraying current is 600-750A, the spraying voltage is 60-75, the main air flow is 30-70 SCFH, and the auxiliary air flow is 3-20 SCFH.
The ultra-high temperature thermal barrier coating of the double-ceramic-layer coating system takes a high-temperature alloy as a matrix, an alloy bonding layer, a nano-structure YSZ ceramic layer and a nano-structure high-entropy cerium zirconate ceramic coating are sequentially arranged on the surface of the matrix, and the nano-structure high-entropy cerium zirconate ceramic coating is prepared by spraying a nano-structure high-entropy cerium zirconate sprayable powder material, wherein:
The superalloy substrate can be one or more of nickel-based, cobalt-based, iron-based and other alloys;
the alloy tie layer may be one or more of NiCrAlY, coCrAlY, niCoCrAlY, niCrAlYCe, coCrAlYCe, niCoCrAlYCe;
The thickness of the alloy bonding layer is 80-200 mu m;
The thickness of the nano-structure YSZ ceramic layer is 70-200 mu m;
the nano-structure high-entropy cerium zirconate ceramic layer is a high-entropy phase and has a thickness of 30-250 mu m.
The preparation method of the ultra-high temperature thermal barrier coating of the double-ceramic-layer coating system comprises the following steps:
Step one, carrying out grinding, polishing and finishing on the surface of a high-temperature alloy matrix, then carrying out sand blasting treatment to ensure that the surface has certain roughness, then carrying out ultrasonic cleaning on the high-temperature alloy matrix by using ethanol, and then preparing an alloy bonding layer (MCrAlY) on the surface by adopting a thermal spraying technology, wherein:
the thermal spray technique may be one of Atmospheric Plasma Spraying (APS), low Pressure Plasma Spraying (LPPS), supersonic flame spraying (HVOF);
The parameters of the atmospheric plasma spraying are as follows: the spraying distance is 100-300 mm, the powder feeding speed is 5-40 g/min, the carrier gas flow is 6-15 SCFH, the spraying current is 450-600A, the spraying voltage is 45-60V, the main air flow is 30-70 SCFH, and the auxiliary air flow is 5-20 SCFH;
Depositing the nano-structure YSZ powder on the surface of the alloy bonding layer obtained in the step one by using an APS technology to obtain the nano-structure YSZ ceramic layer, wherein:
The parameters in the preparation process of the nano-structure YSZ ceramic layer are as follows: the spraying distance is 80-300 mm, the powder feeding speed is 5-25 g/min, the carrier gas flow is 9-14 SCFH, the spraying current is 600-650A, the spraying voltage is 60-65V, the main air flow is 30-55 SCFH, and the auxiliary air flow is 3-15 SCFH;
Step three, depositing nano-structure high-entropy cerium zirconate spherical powder on the surface of the nano-structure YSZ ceramic layer by using an APS technology to form a nano-structure high-entropy cerium zirconate ceramic coating, wherein:
the parameters in the preparation process of the nano-structured high-entropy cerium zirconate ceramic coating are as follows: the spraying distance is 50-250 mm, the powder feeding speed is 5-20 g/min, the carrier gas flow is 8-145 CFH, the spraying current is 600-750A, the spraying voltage is 60-75, the main air flow is 30-70 SCFH, and the auxiliary air flow is 3-20 SCFH.
Compared with the prior art, the invention has the following advantages:
1. the invention utilizes the nanoparticle re-granulation technology to prepare the high-entropy cerium zirconate into the nano-structure spherical powder suitable for thermal spraying for the first time, and provides a method for implementing the high-performance high-entropy material on the thermal spraying nano-structure coating.
2. The invention prepares the nano-structure high-entropy cerium zirconate thermal barrier coating by using the APS technology for the first time, and the technology has the advantages of high energy, wide material application range, convenient operation, high deposition efficiency, easy industrialization and the like. Meanwhile, parameters such as spraying voltage, spraying current, carrier gas flow, powder feeding rate, spraying distance and the like are adjusted to regulate and control the microstructure, porosity and the like of the coating, so that the nano-structure high-entropy cerium zirconate thermal barrier coating with different performance orientations is prepared.
3. The coating prepared by the invention has a typical multi-mode structure, namely, particles which are completely melted, partially melted and unmelted exist, the porosity is 5-15%, and a large number of defects exist in the coating, so that phonon and photon scattering can be increased, thereby reducing the heat conductivity of the coating, relieving the internal stress of the coating and prolonging the service life of the coating.
4. Aiming at different requirements, the invention provides a nano-structure high-entropy cerium zirconate single-ceramic-layer coating system and a YSZ/nano-structure high-entropy cerium zirconate double-ceramic-layer coating system preparation method, which have wider application prospects.
Drawings
FIG. 1 is a process flow for preparing the nano-structured high-entropy cerium zirconate powder and a coating thereof according to the invention;
FIG. 2 is the surface morphology of the nano-powder after granulation;
FIG. 3 is a graph showing the surface morphology and energy spectrum of the granulated powder after heat preservation at 1050 ℃ for 1 h;
FIG. 4 is a graph showing the surface morphology and energy spectrum of the granulated powder after heat preservation at 1300 ℃ for 1 h;
FIG. 5 is an XRD pattern of the granulated powder after 1h incubation at different temperatures;
FIG. 6 is an XRD pattern of a spray coating after different powers;
FIG. 7 is a typical cross-sectional morphology of a high entropy cerium zirconate single ceramic layer coating of the nanostructure LNSGY of example 1;
FIG. 8 is a typical cross-sectional morphology of a high entropy cerium zirconate double ceramic layer coating of the nanostructure LNSGY of example 1;
FIG. 9 is a typical cross-sectional morphology and enlarged region of a nanostructured LNSGY high-entropy cerium zirconate coating.
Detailed Description
The following embodiments are provided to further illustrate the technical scheme of the present invention, but not to limit the technical scheme, and all modifications and equivalent substitutions are included in the scope of the present invention without departing from the spirit and scope of the technical scheme.
Example 1:
The embodiment provides a preparation method of an ultra-high temperature thermal barrier coating of a nano-structure high-entropy cerium zirconate spray powder and a single ceramic layer coating system, as shown in fig. 1, wherein the method is realized by the following steps:
Step one, according to the proportion shown by (La0.2Nd0.2Sm0.2Gd0.2Yb0.2)2(Zr0.75Ce0.25)2O7, weighing nano La 2O3 powder, nano Nd 2O3 powder, nano Sm 2O3 powder, nano Gd 2O3 powder, nano Yb 2O3 powder, nano CeO 2 powder and nano ZrO 2 powder.
Adding deionized water into a vertical ball milling tank, adding ammonium citrate serving as a dispersing agent into the deionized water, adding the raw material powder and zirconia ball grinding balls in the first step after the dispersing agent is completely dissolved, and ball milling for 6 hours to obtain uniform slurry, wherein: the dosage of deionized water is 2 times of the total mass of the raw material powder, the dosage of ammonium citrate is 0.5% of the total mass of the raw material powder, the diameter of the zirconia grinding ball is 3mm and 5mm, and the mass of the zirconia grinding ball is 2.5 times of the mass of the raw material powder.
Adding a binder gum arabic into the uniform slurry obtained in the step two, and ball-milling for 0.5h to obtain uniform slurry, wherein: the consumption of the binder is 2% of the mass of the raw material powder.
Step four, adding the slurry obtained in the step three into a stirrer, conveying the slurry into a drying tower through a peristaltic pump for spray granulation to obtain nano-structure aggregate powder, wherein the step three comprises the following steps: the stirrer parameters were 15 revolutions per minute, spray granulation parameters: the air inlet temperature is 260 ℃, the air outlet temperature is 110 ℃, the needle passing frequency is 15 times per minute, and the peristaltic pump speed is 35-45 revolutions per minute.
Step five, carrying out solid-phase sintering on the nanostructure aggregate powder obtained after the spray granulation in the step four: raising the temperature to 1100-1500 ℃ at 4 ℃/min, preserving the heat for 1h, and optimizing the temperature to be 1200 ℃ according to different process requirements. And then sieving the powder after solid phase sintering by a 200-mesh and 400-mesh sieve to obtain the nano-structure high-entropy cerium zirconate sprayable powder, wherein the phase is a single high-entropy LNSGY phase.
And step six, grinding, polishing and finishing the GH4169 nickel-based superalloy surface by using 40-200 mesh silicon carbide sand paper, then carrying out sand blasting treatment on the substrate surface by using 40-mesh particle brown corundum to ensure that the surface has certain roughness, then carrying out ultrasonic cleaning on the substrate surface by using absolute ethyl alcohol for 1h, and then adopting an atmospheric plasma spraying technology to prepare the NiCrAlY alloy bonding layer on the surface. The preparation parameters of the NiCrAlY alloy bonding layer are as follows: the spraying distance is 120mm, the powder feeding speed is 11.4g/min, the carrier gas flow is 10SCFH, the spraying current is 550A, the spraying voltage is 55V, the main air flow is 50SCFH, the auxiliary air flow is 10SCFH, and the thickness of the bonding layer is 120 mu m.
And step seven, the nano-structure high-entropy cerium zirconate spray-coatable powder obtained in the step five is sprayed and deposited on the surface of the NiCrAlY alloy bonding layer prepared in the step six by adopting atmospheric plasma to form a nano-structure high-entropy cerium zirconate (LNSGY) ceramic coating, so as to obtain the ultrahigh-temperature thermal barrier coating of the single-ceramic-layer coating system. The preparation parameters of the nano-structure high-entropy cerium zirconate ceramic coating are as follows: the spraying distance is 100mm, the powder feeding speed is 9.8g/min, the carrier gas flow is 10SCFH, the spraying current is 690A, the spraying voltage is 65V, the main air flow is 50SCFH, the auxiliary air flow is 10SCFH, and the thickness of the nano-structured high-entropy cerium zirconate ceramic layer is 200 mu m.
Fig. 2 shows the surface morphology of granulated nano La 2O3 powder, nano Nd 2O3 powder, nano Sm 2O3 powder, nano Gd 2O3 powder, nano Yb 2O3 powder, nano CeO 2 powder and nano ZrO 2 powder, and as can be seen from fig. 2, the overall sphericity is good, and the particle size is suitable for plasma spraying.
Fig. 3 shows the surface morphology and energy spectrum of the granulated powder after the powder is insulated for 1h at 1050 ℃, and fig. 3 shows that the nano structure of the powder is well preserved and the elements are uniformly distributed.
Fig. 4 shows the surface morphology and energy spectrum of the granulated powder after heat preservation at 1300 ℃ for 1h, and fig. 4 shows that the nano structure of the powder is well preserved and the elements are uniformly distributed.
FIG. 5 shows XRD patterns of granulated powder after heat preservation for 1h at different temperatures, and FIG. 5 shows that the powder is completed in the high entropy of 1050-1300 ℃ and the high entropy phase is LNSGY.
Fig. 6 shows XRD patterns of spray coating after different powers, and fig. 6 shows that the main phases of the coating are LNSGY, and the phase stability is good.
Fig. 7 shows the typical cross-sectional morphology of the nano-structure LNSGY single ceramic coating of this example, and it can be seen from fig. 7 that the high-entropy single ceramic coating was successfully prepared in this example.
Example 2:
the embodiment provides a preparation method of an ultra-high temperature thermal barrier coating of a nano-structure high-entropy cerium zirconate spray powder and a double-ceramic-layer coating system, as shown in fig. 1, wherein the method is realized by the following steps:
Step one, according to the proportion shown by (La0.2Nd0.2Sm0.2Gd0.2Yb0.2)2(Zr0.75Ce0.25)2O7, weighing nano La 2O3 powder, nano Nd 2O3 powder, nano Sm 2O3 powder, nano Gd 2O3 powder, nano Yb 2O3 powder, nano CeO 2 powder and nano ZrO 2 powder.
Adding deionized water into a vertical ball milling tank, adding a dispersing agent sodium citrate into the deionized water, adding the raw material powder and zirconia ball grinding balls in the step one after the dispersing agent is completely dissolved, and ball milling for 10 hours to obtain uniform slurry, wherein: the dosage of deionized water is 1.8 times of the total mass of the raw material powder, the dosage of sodium citrate is 0.5% of the total mass of the raw material powder, the diameter of the zirconia grinding ball is 3mm and 5mm, and the mass of the zirconia grinding ball is 2 times of the mass of the raw material powder.
Adding a binder gum arabic into the uniform slurry obtained in the step two, and ball-milling for 0.5h to obtain uniform slurry, wherein: the consumption of the binder is 1.5 percent of the mass of the raw material powder.
Step four, adding the slurry obtained in the step three into a stirrer, conveying the slurry into a drying tower through a peristaltic pump for spray granulation to obtain nano-structure aggregate powder, wherein the step three comprises the following steps: the stirrer parameters were 15 revolutions per minute, spray granulation parameters: the air inlet temperature is 250 ℃, the air outlet temperature is 110 ℃, the needle passing frequency is 10 times per minute, and the peristaltic pump speed is 35-45 revolutions per minute.
Step five, carrying out solid-phase sintering on the nanostructure aggregate powder obtained after the spray granulation in the step four: raising the temperature to 1100-1500 ℃ at 4 ℃/min, preserving the heat for 1h, and optimizing the temperature to be 1250 ℃ according to different process requirements. And then sieving the powder after solid phase sintering by a 200-mesh and 400-mesh sieve to obtain the nano-structure high-entropy cerium zirconate sprayable powder, wherein the phase is a single high-entropy LNSGY phase.
And step six, grinding, polishing and finishing the surface of the K417G nickel-based superalloy by using 40-200 mesh silicon carbide sand paper, then carrying out sand blasting treatment on the surface of a matrix by using 40-mesh particle brown corundum to ensure that the surface has certain roughness, then carrying out ultrasonic cleaning on the matrix by using absolute ethyl alcohol for 1h, and then adopting an atmospheric plasma spraying technology to prepare NiCoCrAlYCe alloy bonding layers on the surface of the matrix. The preparation parameters of NiCoCrAlYCe alloy bonding layer are as follows: the spraying distance is 100mm, the powder feeding speed is 12.5g/min, the carrier gas flow is 10SCFH, the spraying current is 530A, the spraying voltage is 53V, the main air flow is 48SCFH, the auxiliary air flow is 12SCFH, and the thickness of the bonding layer is 100 mu m.
And step seven, taking nano-structure YSZ powder, and adopting atmospheric plasma spraying to deposit on the surface of the NiCoCrAlYCe alloy bonding layer prepared in the step six. The preparation parameters of the YSZ ceramic coating are as follows: the spraying distance is 140mm, the powder feeding rate is 15g/min, the carrier gas flow is 10SCFH, the spraying current is 620A, the spraying voltage is 62V, the main air flow is 52SCFH, the auxiliary air flow is 11SCFH, and the thickness of the ceramic layer is 150 mu m.
And step eight, the nano-structure high-entropy cerium zirconate sprayable powder screened in the step five is sprayed and deposited on the surface of the YSZ layer prepared in the step seven by adopting atmospheric plasma to form a nano-structure high-entropy cerium zirconate (LNSGY) ceramic coating, so as to obtain the ultra-high temperature thermal barrier coating of the double-ceramic-layer coating system. The preparation parameters of LNSGY ceramic coating are: the spraying distance is 90mm, the powder feeding speed is 9.5g/min, the carrier gas flow is 10SCFH, the spraying current is 700A, the spraying voltage is 66V, the main air flow is 49SCFH, the auxiliary air flow is 11SCFH, and the thickness of the ceramic layer is 50 mu m, so that the double ceramic coating can be obtained.
FIG. 8 is a typical cross-sectional morphology of a dual ceramic coating with nanostructures LNSGY according to this example
Example 3:
The embodiment provides a preparation method of a nano-structure high-entropy cerium zirconate spray powder and a coating, which is realized by the following steps:
Step one, according to the proportion shown by (Yb0.2Eu0.2Tb0.2Dy0.2Lu0.2)2(Zr0.5Ce0.5)2O7, weighing nano Yb 2O3 powder, nano Eu 2O3 powder, nano Tb 2O3 powder, nano Dy 2O3 powder, nano Lu 2O3 powder, ceO 2 powder and nano ZrO 2 powder.
Adding deionized water into a vertical ball milling tank, adding ammonium citrate serving as a dispersing agent into the deionized water, adding the raw material powder and zirconia ball grinding balls in the first step after the dispersing agent is completely dissolved, and performing ball milling for 12 hours to obtain uniform slurry, wherein: the dosage of deionized water is 2 times of the total mass of the raw material powder, the dosage of ammonium citrate is 0.5% of the total mass of the raw material powder, the diameter of the zirconia grinding ball is 3mm and 5mm, and the mass of the zirconia grinding ball is 2.5 times of the mass of the raw material powder.
Adding a binder gum arabic into the uniform slurry obtained in the step two, and ball-milling for 0.5h to obtain uniform slurry, wherein: the consumption of the binder is 1.0 percent of the mass of the raw material powder.
Step four, adding the slurry obtained in the step three into a stirrer, conveying the slurry into a drying tower through a peristaltic pump for spray granulation to obtain nano-structure aggregate powder, wherein the step three comprises the following steps: the stirrer parameters were 15 revolutions per minute, spray granulation parameters: the air inlet temperature is 245 ℃, the air outlet temperature is 120 ℃, the needle passing frequency is 10 times per minute, and the peristaltic pump speed is 30-45 revolutions per minute.
Step five, carrying out solid-phase sintering on the nanostructure aggregate powder obtained after the spray granulation in the step four: raising the temperature to 950-1650 ℃ at 5 ℃/min, preserving the heat for 1h, and optimizing the temperature to be 1150 ℃ according to different process requirements. And then sieving the powder after solid phase sintering by a 200-mesh and 400-mesh sieve to obtain the nano-structure high-entropy zirconate sprayable powder, wherein the phase is a single high-entropy phase.
Step six, grinding, polishing and finishing the GH4169 nickel-based superalloy surface by using 40-200 mesh silicon carbide sand paper, then carrying out sand blasting treatment on the substrate surface by using 60-mesh particle brown corundum to ensure that the surface has certain roughness, respectively carrying out ultrasonic cleaning on the substrate surface by using absolute ethyl alcohol and acetone for 30min, and then preparing the NiCrAlY alloy bonding layer on the surface by adopting a supersonic flame spraying technology. The preparation parameters of the NiCrAlY alloy bonding layer are as follows: the spraying distance is 240mm, the powder feeding rate is 30g/min, the carrier gas flow is 5NLPM, the shielding gas flow is 360NLPM, the gas flow is 180NLPM, the oxygen flow is 240NLPM, and the thickness of the NiCrAlY alloy bonding layer is 100 μm.
And step seven, the nano-structure high-entropy zirconate sprayable powder screened in the step five is deposited on the surface of the NiCrAlY alloy bonding layer prepared in the step six by adopting atmospheric plasma spraying to form a nano-structure high-entropy cerium zirconate (LNSGY) ceramic coating, and an ultrahigh-temperature thermal barrier coating of a single-ceramic-layer coating system is obtained. The preparation parameters of the ceramic coating are as follows: the spraying distance is 110mm, the powder feeding speed is 9.0g/min, the carrier gas flow is 9SCFH, the spraying current is 700A, the spraying voltage is 70V, the main air flow is 55SCFH, the auxiliary air flow is 11SCFH, and the thickness of the ceramic layer is 200 mu m.
Example 4:
This example is different from examples 1-3 in that: the chemical formula of the nano-structured high-entropy cerium zirconate spray powder is (Sm0.2Y0.2Yb0.2 Dy0.2Gd0.2)2(Zr0.8Ce0.2)2O7.
Example 5:
This example is different from examples 1-3 in that: the chemical formula of the nano-structured high-entropy cerium zirconate spray powder is (La0.2Sm0.2Y0.2Yb0.2 Lu0.2 Tm0.2)2(Zr0.25Ce0.75)2O7.
Example 6:
This example is different from examples 1-3 in that: the chemical formula of the nano-structured high-entropy cerium zirconate spray powder is (Eu0.2Gd0.2Y0.2Yb0.2 Tb0.2 Lu0.2Tm0.2)2(Zr0.9Ce0.1)2O7.
Claims (10)
1. A nano-structure high-entropy cerium zirconate powder material capable of being sprayed is characterized in that the powder material capable of being sprayed is A 2B2O7 type zirconate, wherein A consists of 5-10 elements in La, nd, sm, gd, yb, eu, tb, dy, lu, Y, tm, and B consists of Zr and Ce.
2. A method for preparing the nanostructured high entropy cerium zirconate sprayable powder material according to claim 1, comprising the steps of:
Step one, weighing nano A 2O3 powder raw materials and nano B 2O3 powder raw materials according to a stoichiometric ratio shown in a chemical formula A 2B2O7, wherein: the A 2O3 powder raw materials are 5-10 of nano La 2O3 powder, nano Nd 2O3 powder, nano Sm 2O3 powder, nano Gd 2O3 powder, nano Yb 2O3 powder, nano Eu 2O3 powder, nano Tb 2O3 powder, nano Dy 2O3 powder, nano Lu 2O3 powder, nano Y 2O3 powder and nano Tm 2O3 powder; the nano B 2O3 powder raw materials are nano CeO 2 powder and nano ZrO 2 powder;
Adding deionized water into a ball mill, adding a dispersing agent into the deionized water, adding the nano powder raw material in the first step after the dispersing agent is completely dissolved, performing ball milling, adding a binder to obtain uniform slurry, and performing spray granulation and solid-phase sintering to obtain nano-structure high-entropy cerium zirconate spherical powder, wherein: the dosage of the deionized water is 0.5-2 times of the total mass of the used nano powder raw materials, the dosage of the dispersing agent is 0.05-5% of the total mass of the nano powder raw materials, and the binder is 0.05-10% of the total mass of the nano powder raw materials.
3. The method for preparing the nano-structured high-entropy cerium zirconate spray-coating powder material according to claim 2, wherein the particle sizes of the nano La 2O3 powder, the nano Nd 2O3 powder, the nano Sm 2O3 powder, the nano Gd 2O3 powder, the nano Yb 2O3 powder, the nano Eu 2O3 powder, the nano Tb 2O3 powder, the nano Dy 2O3 powder, the nano Lu 2O3 powder, the nano Y 2O3 powder, the nano Tm 2O3 powder, the nano CeO 2 powder and the nano ZrO 2 powder are all 10-80 nm; the dispersing agent is one or more of sodium tripolyphosphate, sodium hexametaphosphate, ammonium citrate and sodium citrate; the binder is one of gum arabic, polyvinyl alcohol, carboxymethyl cellulose and epoxy resin; the nano-structure high-entropy cerium zirconate spherical powder is a high-entropy phase with the grain size smaller than 100 nm; the diameter of the zirconia grinding ball is 3-8 mm, the mass of the zirconia grinding ball is 1-3 times of the total mass of the nano powder raw material, the ball milling time is 4-12 h, and the revolution is 400-1000 rpm; the solid phase sintering is carried out in an atmospheric environment, and the conditions of the solid phase sintering are as follows: heating to 1100-1600 ℃ at the speed of 1-15 ℃/min, and preserving heat for 0.5-3 h.
4. The ultra-high temperature thermal barrier coating of the single ceramic layer coating system is characterized in that the coating takes a high-temperature alloy as a matrix, an alloy bonding layer and a nano-structure high-entropy cerium zirconate ceramic coating are sequentially arranged on the surface of the matrix, and the nano-structure high-entropy cerium zirconate ceramic coating is prepared by spraying the nano-structure high-entropy cerium zirconate sprayable powder material according to claim 1.
5. The ultra-high temperature thermal barrier coating of the single ceramic layer coating system of claim 4, wherein the superalloy substrate is one or more of a nickel-based, cobalt-based, iron-based alloy; the alloy bonding layer is one or more of NiCrAlY, coCrAlY, niCoCrAlY, niCrAlYCe, coCrAlYCe, niCoCrAlYCe, and the thickness of the alloy bonding layer is 80-200 mu m; the nano-structure high-entropy cerium zirconate ceramic layer is a high-entropy phase and has a thickness of 30-250 mu m.
6. A method for producing an ultra-high temperature thermal barrier coating of a single ceramic layer coating system according to any one of claims 4 to 5, characterized in that the method comprises the steps of:
firstly, performing grinding, polishing and finishing on the surface of a high-temperature alloy matrix, performing sand blasting treatment to ensure that the surface has certain roughness, performing ultrasonic cleaning on the high-temperature alloy matrix by using ethanol, and preparing an alloy bonding layer on the surface by adopting a thermal spraying technology;
and step two, depositing the nano-structure high-entropy cerium zirconate spherical powder on the surface of the alloy bonding layer obtained in the step one by utilizing an atmospheric plasma spraying technology to form the nano-structure high-entropy cerium zirconate ceramic coating.
7. The method for preparing the ultra-high temperature thermal barrier coating of the single ceramic layer coating system according to claim 6, wherein the thermal spraying technology is one of atmospheric plasma spraying, low-pressure plasma spraying and supersonic flame spraying; the parameters in the preparation process of the nano-structured high-entropy cerium zirconate ceramic coating are as follows: the spraying distance is 50-250 mm, the powder feeding speed is 5-20 g/min, the carrier gas flow is 8-145 CFH, the spraying current is 600-750A, the spraying voltage is 60-75, the main air flow is 30-70 SCFH, and the auxiliary air flow is 3-20 SCFH.
8. The ultra-high temperature thermal barrier coating of the double-ceramic-layer coating system is characterized in that the coating takes a high-temperature alloy as a substrate, an alloy bonding layer, a nano-structure YSZ ceramic layer and a nano-structure high-entropy cerium zirconate ceramic coating are sequentially arranged on the surface of the substrate, and the nano-structure high-entropy cerium zirconate ceramic coating is prepared by spraying the nano-structure high-entropy cerium zirconate sprayable powder material according to claim 1.
9. The ultra-high temperature thermal barrier coating of the dual ceramic layer coating system of claim 8, wherein the superalloy substrate may be one or more of nickel-based, cobalt-based, iron-based alloys; the alloy tie layer may be one or more of NiCrAlY, coCrAlY, niCoCrAlY, niCrAlYCe, coCrAlYCe, niCoCrAlYCe; the thickness of the alloy bonding layer is 80-200 mu m; the thickness of the nano-structure YSZ ceramic layer is 70-200 mu m; the nano-structure high-entropy cerium zirconate ceramic layer is a high-entropy phase and has a thickness of 30-250 mu m.
10. A method for preparing an ultra-high temperature thermal barrier coating of a dual ceramic layer coating system according to any one of claims 8 to 9, characterized in that the method comprises the steps of:
firstly, performing grinding, polishing and finishing on the surface of a high-temperature alloy matrix, performing sand blasting treatment to ensure that the surface has certain roughness, performing ultrasonic cleaning on the high-temperature alloy matrix by using ethanol, and preparing an alloy bonding layer on the surface by adopting a thermal spraying technology;
depositing the nano-structure YSZ powder on the surface of the alloy bonding layer obtained in the first step by using an APS technology to obtain a nano-structure YSZ ceramic layer;
And thirdly, depositing the nano-structure high-entropy cerium zirconate spherical powder on the surface of the nano-structure YSZ ceramic layer by using an APS technology to form the nano-structure high-entropy cerium zirconate ceramic coating.
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