CN114804898A - Multi-component co-doped zirconia thermal barrier coating material and preparation method thereof - Google Patents
Multi-component co-doped zirconia thermal barrier coating material and preparation method thereof Download PDFInfo
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Abstract
The embodiment of the invention discloses a multi-element co-doped zirconia thermal barrier coating material and a preparation method thereof, wherein the material comprises the following materials in mole fraction: 0.66 percent of zirconium oxide, 0.095 to 0.100 percent of trivalent rare earth oxide and pentavalent oxide respectively, and the molar ratio of the trivalent rare earth oxide to the pentavalent oxide is equal. The invention has excellent CMAS lava corrosion resistance and is expected to be used as a new generation of thermal barrier coating material with higher service temperature.
Description
Technical Field
The invention relates to the field of materials, in particular to a multi-element co-doped zirconia thermal barrier coating material and a preparation method thereof.
Background
Thermal Barrier Coatings (TBCs) are the core technology for aircraft engine turbine blades, and ceramic Thermal barriers with low Thermal conductivity reduce the surface temperature of superalloy components, making it possible to service superalloys in environments close to or above their melting point temperature. The ceramic thermal insulation layer widely used and studied at present is 6-8wt% Y 2 O 3 Stabilized ZrO 2 (7 YSZ) and good comprehensive properties (mechanical property and thermal property) make the ceramic material stand out from other ceramic materials.
However, with the increasing of the service temperature of the engine, the combustion chamber is rich in CaO-MgO-Al due to the entry of micro-dust and engine abrasive dust in the air 2 O 3 -SiO 2 (CMAS) deposits and melts on the surface of the blade, and severe chemical attack occurs on the 7YSZ, so that the blade is causedThe 7YSZ coating powderizes, accelerating its peel failure, eventually exposing the high temperature components directly to temperatures above their melting point with severe consequences. Therefore, how to realize excellent CMAS molten rock corrosion resistance and protect high-temperature alloy components from being corroded by CMAS molten salt on the premise of not changing basic characteristics (high temperature resistance, thermal physical property and thermal shock resistance) of the thermal barrier coating is a key direction of research of scientists in various countries at present.
Disclosure of Invention
The technical problem to be solved by the embodiment of the invention is to provide a multi-element co-doped zirconia thermal barrier coating material and a preparation method thereof, so that the excellent CMAS lava corrosion resistance is realized on the premise of not changing the basic characteristics of the thermal barrier coating, and a high-temperature alloy part is protected from being corroded by CMAS molten salt.
In order to solve the technical problem, the embodiment of the invention provides a multi-element co-doped zirconia thermal barrier coating material which comprises the following materials in mole fraction: 0.66 percent of zirconium oxide, 0.095 to 0.100 percent of trivalent rare earth oxide and pentavalent oxide respectively, and the molar ratio of the trivalent rare earth oxide to the pentavalent oxide is equal.
Correspondingly, the embodiment of the invention also provides a preparation method of the multi-element co-doped zirconia thermal barrier coating material, which comprises the following steps:
step 1: adding raw materials into a nylon ball milling tank, carrying out planetary ball milling by using zirconium oxide as a grinding body and isopropanol as a ball milling medium to uniformly mix raw material powder to obtain mixed powder, wherein the raw materials comprise the following materials in molar fraction: 0.66 percent of zirconium oxide, 0.095 to 0.100 percent of trivalent rare earth oxide and pentavalent oxide respectively, and the trivalent rare earth oxide and the pentavalent oxide are in equal molar ratio;
step 2: drying the mixed powder, grinding, sieving by a 400-mesh sieve, and pressing into a pre-sintered block by single-shaft cold pressing under 150-200 MPa;
and step 3: and (3) carrying out heat treatment on the pre-sintered block at the temperature of 1500-1700 ℃ for 10-20 hours in an air environment, and obtaining the multi-element co-doped zirconia thermal barrier coating material through high-temperature solid-phase reaction.
Further, the particle size of each oxide powder in the raw material powder is 100-500 nm.
Further, in the step 1, the rotation speed of the nylon ball milling tank is 300-.
The invention has the following beneficial effects:
1. the invention obtains the multi-element rare earth co-doped zirconia thermal barrier coating material with CMAS lava corrosion resistance by doping trivalent rare earth oxide (yttrium oxide or ytterbium oxide or lanthanum oxide) and pentavalent oxide (niobium oxide and tantalum oxide) with high molar and high content on a zirconia base through high-temperature solid-phase reaction.
2. The CMAS lava corrosion experiment shows that the material has higher reaction activity with CMAS molten salt: the corrosion inhibitor is dissolved and re-precipitated in CMAS lava corrosion at 1300 ℃ to form a compact reaction product, thereby effectively preventing further corrosion of the CMAS lava.
3. The material obtained by the invention can improve phonon or photon diffraction due to the defect introduced by high doping, thereby having lower thermal conductivity (about 1.5 W.m < -1 > K < -1 >) and thermal expansion coefficient (11.2 ppm < -1 >). In addition, the ternary and quinary oxide equimolar codoped material also has good mechanical properties (the elastic modulus is about 150 GPa, the fracture toughness is about 3-4 MPa.m1/2) and high-temperature stability, and is a TBC material with great potential for resisting CMAS molten salt corrosion.
Drawings
FIG. 1 is a graph of the X-ray diffraction results of a sample of the multi-component co-doped zirconia thermal barrier coating material of example 1 of the present invention.
FIG. 2 is an SEM photograph of the surface of a sample of the multi-component co-doped zirconia thermal barrier coating material of example 1 of the present invention after hot corrosion.
FIG. 3 is a cross-sectional SEM photograph of a multi-component co-doped zirconia thermal barrier coating material compact sample of example 2 of the invention after 24 hours of CMAS corrosion.
FIG. 4 shows the variation of the corrosion depth of the multi-doped zirconia thermal barrier coating material sample and CMAS lava with reaction time in example 2 of the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application can be combined with each other without conflict, and the present invention is further described in detail with reference to the drawings and specific embodiments.
The multi-element co-doped zirconia thermal barrier coating material disclosed by the invention comprises the following materials in mole fraction: zirconia 0.66, trivalent rare earth oxide (yttria Y) 2 O 3 Yb of ytterbium oxide 2 O 3 Or lanthanum oxide La 2 O 3 ) With pentavalent oxide (niobium oxide Nb) 2 O 3 Or tantalum oxide Ta 2 O 3 ) 0.095-0.100 of each, and the molar ratio of the trivalent rare earth oxide to the pentavalent oxide is equal.
Aiming at the problem that the traditional thermal barrier coating 7YSZ is easily corroded by CMAS molten salt, the invention carries out multielement doping on the basis of the same zirconia matrix, so that the coating has good compatibility with 7YSZ and can be used as a 7YSZ outer protection layer to resist the CMAS molten salt corrosion. The material has high CMAS reaction activity due to high-content oxide doping, so that a compact reaction product is easy to precipitate to inhibit CMAS corrosion, and the equimolar doped zirconia of a ternary oxide (yttrium oxide, ytterbium oxide or lanthanum oxide) and a quinary oxide (niobium oxide or tantalum oxide) can avoid the generation of oxygen vacancies, reduce the element segregation effect and avoid the grain boundary corrosion of the material due to CMAS.
Example 1:
weighing ZrO according to calculation 2 41.74g、Y 2 O 3 19.70g、Ta 2 O 3 38.36g of the powder was put into a nylon ball mill pot of a planetary ball mill, and planetary ball milling was carried out using zirconia as a milling body and isopropanol as a ball milling medium. The powder was dried, sieved (400 mesh) and compression molded by uniaxial cold pressing under 150 MPa. Placing the pre-sintered block into a high-temperature furnace, pre-sintering to 1500 ℃, preserving heat for 20 hours, cooling along with the furnace, taking out to obtain a multi-element co-doped zirconia thermal barrier coating material ZYTO, wherein the ZYTO prepared by the method is in a single tetragonal phase and has a pure phase and no impurity phase as shown in figure 1 and an X-ray diffraction pattern,and the grain radius is about 3-5 microns in size.
CMAS powder is coated on the surface of a multi-element co-doped zirconia thermal barrier coating material ZYN block prepared by the invention, and the component of the CMAS powder is 33CaO-9MgO-13Al 2 O 3 -45SiO 2 (molar ratio) and a coating density of 20. + -.2 mg/cm 2 The samples with the coated CMAS powder were placed in a high temperature oven at 1300 ℃ for various times of 1-100 hours at constant temperature. After the CMAS molten salt acts, a compact crystal layer with the main component of zirconia is formed on the surface of the ZYTO, as shown in figure 2, which shows that the multi-element co-doped zirconia thermal barrier coating material ZYTO prepared by the invention has excellent CMAS molten rock corrosion resistance.
Example 2:
weighing ZrO according to calculation 2 49.32g、Y 2 O 3 23.28g、Nb 2 O 3 27.40g of the powder is put into a nylon ball milling tank of a planetary ball mill, and planetary ball milling is carried out by taking zirconium oxide as a grinding body and isopropanol as a ball milling medium. The powder was dried, sieved (400 mesh) and compression molded by cold uniaxial pressing at 150 MPa. And (3) placing the pre-sintered block into a high-temperature furnace, pre-sintering to 1500 ℃, preserving heat for 10 hours, cooling along with the furnace, and taking out to obtain the multi-element co-doped zirconia thermal barrier coating material ZYNO.
CMAS powder is coated on the surface of a multi-element co-doped zirconia thermal barrier coating material ZYNO block prepared by the invention, and the component of the CMAS powder is 33CaO-9MgO-13Al 2 O 3 -45SiO 2 (molar ratio) and a coating density of 20. + -.2 mg/cm 2 The samples with the coated CMAS powder were placed in a high temperature oven at 1300 ℃ for various times of 1-100 hours at constant temperature. After the CMAS molten salt acts, a compact crystallization layer (the corrosion time is 24 hours in figure 3) with the main component of zirconia is formed on the surface of the ZYNO, and the CMAS molten salt can be effectively prevented from further reacting with a matrix. In addition, as shown in fig. 4, the change of the corrosion depth of the CMAS lava in the ZYNO block along with the reaction time shows that the corrosion depth of the ZYNO block is parabolic, which fully shows that the polynary co-doped zirconia thermal barrier coating material ZYNO prepared by the invention has excellent CMAS lava corrosion resistance.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. The multi-element co-doped zirconia thermal barrier coating material is characterized by comprising the following materials in mole fraction: 0.66 percent of zirconium oxide, 0.095 to 0.100 percent of trivalent rare earth oxide and pentavalent oxide respectively, and the molar ratio of the trivalent rare earth oxide to the pentavalent oxide is equal.
2. A preparation method of a multi-element co-doped zirconia thermal barrier coating material is characterized by comprising the following steps:
step 1: adding raw materials into a nylon ball milling tank, carrying out planetary ball milling by using zirconium oxide as a grinding body and isopropanol as a ball milling medium to uniformly mix raw material powder to obtain mixed powder, wherein the raw materials comprise the following materials in molar fraction: 0.66 percent of zirconium oxide, 0.095 to 0.100 percent of trivalent rare earth oxide and pentavalent oxide respectively, and the trivalent rare earth oxide and the pentavalent oxide are in equal molar ratio;
and 2, step: drying the mixed powder, grinding, sieving by a 400-mesh sieve, and pressing into a pre-sintered block by single-shaft cold pressing under 150-200 MPa;
and step 3: and (3) carrying out heat treatment on the pre-sintered block at the temperature of 1500-1700 ℃ for 10-20 hours in an air environment, and obtaining the multi-element co-doped zirconia thermal barrier coating material through high-temperature solid-phase reaction.
3. The method for preparing the multi-element co-doped zirconia thermal barrier coating material as claimed in claim 2, wherein the particle size of each oxide powder in the raw material powder is 100-500 nm.
4. The method for preparing the multi-element co-doped zirconia thermal barrier coating material as claimed in claim 2, wherein in the step 1, the rotation speed of the nylon ball milling tank is 300-600 rpm, the ball milling time is 24-96 hours, and the ball milling process is stopped for 20 minutes per hour to prevent the temperature from being too high.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050064225A1 (en) * | 2003-08-07 | 2005-03-24 | Snecma Moteurs | Thermal barrier composition, a superalloy machine part provided with a coating having such a composition, a ceramic coating, and a method of fabricating the coating |
| CN101397214A (en) * | 2008-11-05 | 2009-04-01 | 内蒙古科技大学 | Multi-element co-stabilizing zirconia of heat barrier coat material and preparation method |
| CN103130501A (en) * | 2013-03-22 | 2013-06-05 | 西北有色金属研究院 | Multi-element stable zirconium oxide corrosion-resistant thermal barrier coating material |
| CN113773075A (en) * | 2021-09-22 | 2021-12-10 | 湘潭大学 | CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof |
| CN113816751A (en) * | 2021-09-01 | 2021-12-21 | 华东理工大学 | Tetragonal phase high-entropy thermal barrier coating material and preparation method thereof |
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- 2022-04-22 CN CN202210429852.7A patent/CN114804898A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050064225A1 (en) * | 2003-08-07 | 2005-03-24 | Snecma Moteurs | Thermal barrier composition, a superalloy machine part provided with a coating having such a composition, a ceramic coating, and a method of fabricating the coating |
| CN101397214A (en) * | 2008-11-05 | 2009-04-01 | 内蒙古科技大学 | Multi-element co-stabilizing zirconia of heat barrier coat material and preparation method |
| CN103130501A (en) * | 2013-03-22 | 2013-06-05 | 西北有色金属研究院 | Multi-element stable zirconium oxide corrosion-resistant thermal barrier coating material |
| CN113816751A (en) * | 2021-09-01 | 2021-12-21 | 华东理工大学 | Tetragonal phase high-entropy thermal barrier coating material and preparation method thereof |
| CN113773075A (en) * | 2021-09-22 | 2021-12-10 | 湘潭大学 | CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof |
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