CN113773075B - CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof - Google Patents
CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof Download PDFInfo
- Publication number
- CN113773075B CN113773075B CN202111104975.5A CN202111104975A CN113773075B CN 113773075 B CN113773075 B CN 113773075B CN 202111104975 A CN202111104975 A CN 202111104975A CN 113773075 B CN113773075 B CN 113773075B
- Authority
- CN
- China
- Prior art keywords
- temperature
- hours
- coating material
- powder
- coating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—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
- C04B35/495—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 vanadium, niobium, tantalum, molybdenum or tungsten oxides or solid solutions thereof with other oxides, e.g. vanadates, niobates, tantalates, molybdates or tungstates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6565—Cooling rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9669—Resistance against chemicals, e.g. against molten glass or molten salts
-
- 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
Abstract
The invention discloses a CMAS erosion resistant zirconium-tantalum thermal barrier coating material and a preparation method thereof, wherein the coating material comprises Zr element, Y element, ta element and O element, and ZrO 2 The amount of the component may further comprise m-YTaO, in an amount ranging from 0 to 60mol.%, based on the total mass of the material 4 t-ZrO 2 . Compared with the traditional yttria-stabilized zirconia (YSZ) coating, the coating material prepared by the invention has smaller thickness of a reaction layer and phase change degree after CMAS corrosion in the same environment, and has better CMAS corrosion resistance.
Description
Technical Field
The invention relates to the technical field of thermal barrier coatings, in particular to the technical field of zirconium-tantalum thermal barrier coatings.
Background
Thermal barrier coatings (Thermal Barrier Coatings, TBCs for short) are currently one of the most practical solutions capable of greatly increasing the operating temperature of an aircraft engine. The TBCs commonly used at present are zirconium oxide (6-8 YSZ) doped with 7+/-1 wt.% yttrium oxide, and have the advantages of low thermal conductivity, proper thermal expansion coefficient, higher fracture toughness and the like, but as the engine is developed towards high thrust-weight ratio, the inlet temperature before the turbine is continuously increased, the surface temperature of the blade is close to 1400 ℃, and when the coating is in an ultra-high temperature environment above 1300 ℃, the supersaturated tetragonal phase (t' phase) ZrO in YSZ is diffused along with the diffusion of yttrium element 2 Will undergo martensitic transformation to form monoclinic (m-phase) ZrO 2 And a volume expansion of 3-6% is generated, resulting in stress in the interior of the coating to form cracks; meanwhile, when the service temperature of the coating is higher than 1200 ℃, the garment is takenCaO, mgO, al in service environment 2 O 3 SiO (silicon oxide) 2 Particles or deposits (collectively referred to as CMAS) that are the major component inevitably infiltrate and corrode the coating, the zirconium and yttrium elements of the coating will co-dissolve in the melt, resulting in yttrium-depleted regions at the interface of the coating and CMAS, decreasing the phase stability of the coating, while zirconium has a solubility in CMAS less than yttrium, resulting in partially yttrium-depleted ZrO 2 The particles are re-precipitated, and the mechanical property and the phase stability of the material are reduced along with the spheroidization and the occurrence of t-to-m phase transformation, and the parameters such as the elastic modulus, the thermal expansion coefficient and the like of the material are changed. Therefore, the development of novel ultra-high temperature thermal barrier coating materials is an important and urgent need.
Disclosure of Invention
The invention aims to provide a novel zirconium-tantalum thermal barrier coating material and a preparation method thereof, and the material has smaller CMAS reaction layer thickness, stronger CMAS corrosion resistance and high-temperature stability compared with the thermal barrier coating materials in the prior art, such as YSZ thermal barrier coating materials and the like.
The technical scheme of the invention is as follows:
a zirconium-tantalum thermal barrier coating material comprises Zr element, Y element, ta element and O element, wherein the content of substances is 0-60 mol%ZrO 2 。
According to some preferred embodiments of the invention, the zirconium tantalum based thermal barrier coating material comprises the component m-YTaO 4 And t-ZrO 2 。
In the preferred embodiment, m and t represent monoclinic and tetragonal crystal structures, respectively.
According to some preferred embodiments of the present invention, the atomic ratio of Ta, Y, zr in the components of the zirconium tantalum based thermal barrier coating material is 1:1: (0.5-3).
The invention further provides a method for preparing the zirconium-tantalum thermal barrier coating material, which comprises the following steps:
respectively dissolving a non-oxide raw material containing Ta element, an oxide raw material containing Y element and an oxide raw material containing Zr element according to the proportioning requirements to obtain corresponding raw material solutions;
mixing the obtained raw material solutions, adding the mixture into ammonia water, reacting to obtain colloidal precipitate, separating the colloidal precipitate, and performing first drying to obtain precipitate powder;
sintering the precipitated powder at a first high temperature of 1500-1700 ℃ for 10-15 hours to obtain first sintered powder;
and ball-milling the first sintered powder, and performing second drying and heating activation on the obtained ball-milled powder to obtain the coating material powder.
According to some preferred embodiments of the invention, the method of preparing further comprises: and carrying out static pressure molding on the coating material powder, and carrying out second high-temperature sintering at 1500-1700 ℃ on the molded body to obtain the coating material block.
According to some preferred embodiments of the invention, the second high temperature sintering process comprises: the molded body is heated to 300 ℃ at the temperature of 80 ℃ and 100 ℃ and 150 ℃ respectively for 20-40 minutes at the temperature rising rate of 5-15 ℃/min, then heated to 600 ℃ at the temperature rising rate of 0.5-1.5 ℃/min and kept for 1.5-2.5 hours, then heated to 1600 ℃ at the temperature rising rate of 5-15 ℃/min and kept for 15-25 hours, and cooled to 300 ℃ at the temperature reducing rate of 0.5-1.5 ℃/min after the heat preservation is completed, and then naturally cooled.
According to some preferred embodiments of the invention, the shaping is carried out at a pressure of 500-700 mpa and/or for a time of 5-10 minutes.
According to some preferred embodiments of the invention, the first drying is at a temperature of 70-90 ℃ and/or for a time of 20-50 hours.
According to some preferred embodiments of the invention, the second drying is at a temperature of 70-90 ℃ and/or for a time of 5-15 hours.
According to some preferred embodiments of the invention, the aqueous ammonia has a pH of not less than 10.
According to some preferred embodiments of the invention, the activation is carried out at a temperature of 300-500 ℃ and/or for a time period of 1-3 hours.
According to some preferred embodiments of the present invention, the medium for ball milling is absolute ethanol, the ball milling frequency is 20-40Hz, and the ball milling time is 10-15 hours.
According to some preferred embodiments of the invention, the non-oxide containing Ta element is selected from TaCl 5 The oxide containing Y element is selected from Y (NO) 3 ) 3 ·6H 2 O, the oxide containing Zr element is selected from ZrO (NO 3 ) 2 。
According to some preferred embodiments of the invention, the solvent of the raw material solution is selected from absolute ethanol and/or distilled water
The coating material contains zirconium element, tantalum element, yttrium element and oxygen element, wherein the tantalum material formed by the tantalum element has the characteristics of low heat conductivity, thermal expansion coefficient matched with a metal substrate, higher fracture toughness, high-temperature phase stability and the like, and is oriented to ZrO 2 The stable t' phase at the ultra-high temperature of 1500 ℃ can be obtained after co-doping yttrium and tantalum elements, the heat conductivity and hardness of the coating can be reduced, meanwhile, yttrium and tantalum can form YTaO with lower heat conductivity, higher fracture toughness, t phase transformation temperature of about 1430 ℃ and smaller volume change compared with YSZ 4 After the multi-component cooperation, the use temperature of the coating material can reach more than 1600 ℃, and the high-temperature deformation is small and the high-temperature stability is good.
In addition, the co-doping of yttrium and tantalum in the coating material of the invention can greatly improve the ZrO 2 The solubility of yttrium in CMAS is reduced, and the addition of tantalum element can reduce the activity of yttrium in the coating, which plays a role in stabilization, and reduce the enrichment of yttrium into CMAS, thereby improving the stability of the coating; the inventors have further found that CMAS cannot fully wet YTaO of the present coating material at high temperatures 4 The surface of the coating obviously reduces the thickness of the reaction layer of the coating, has better corrosion resistance, and simultaneously discovers that ZrO 2 -Ta 2 O 5 -Y 2 O 3 After the coating is corroded, no spheroidization phenomenon occurs at a solid-liquid interface, regular and compact corrosion products are formed, and the degree of yttrium deficiency of the coating is greatly reduced compared with YSZ.
Drawings
FIG. 1 is a flow chart of a specific zirconium tantalum coating preparation;
FIG. 2 is an XRD diffraction pattern of a particular sample block of zirconium tantalum based coating;
FIG. 3 is a topography of the zirconium tantalum coated block obtained in example 1;
FIG. 4 is a graph showing comparison of the morphology of the reaction layer and the corrosion interface after CMAS corrosion for 4 hours for (a) a YSZ sample and (b) a zirconium tantalum based coating sample of example 1;
FIG. 5 is a graph comparing the morphology of the etched interface after CMAS etching for 4 hours for (a) YSZ samples and (b) zirconium tantalum based coatings in example 2.
Detailed Description
The present invention will be described in detail with reference to the following examples and drawings, but it should be understood that the examples and drawings are only for illustrative purposes and are not intended to limit the scope of the present invention in any way. All reasonable variations and combinations that are included within the scope of the inventive concept fall within the scope of the present invention.
Referring to FIG. 1, a specific method for preparing a zirconium tantalum thermal barrier coating comprises:
TaCl as raw material 5 Dissolving in absolute ethanol, Y (NO) 3 ) 3 ·6H 2 O、ZrO(NO 3 ) 2 Respectively dissolving in distilled water and/or absolute ethyl alcohol;
mixing the raw material solutions, and then dropwise adding the mixed raw material solutions into ammonia water to obtain white colloidal precipitates which are uniformly distributed;
centrifuging the precipitate, washing with distilled water, vacuum filtering, and drying to obtain precipitate powder;
placing the obtained powder into a sintering furnace for first high-temperature sintering, and then performing ball milling, second drying and heating activation to obtain the required nanoscale coating powder;
and physically briquetting the obtained coating powder under a static pressure machine through a die, and obtaining a crystallized coating block with uniform components after second high-temperature sintering.
Some preferred embodiments thereof include:
the solvent used for dissolution is selected from absolute ethanol and/or distilled water.
The pH value of the ammonia water is not less than 10.
The temperature of the first drying is 70-90 ℃ and the drying time is 20-50 hours.
The temperature of the first high-temperature sintering is 1500-1700 ℃, and the sintering time is 10-15 hours.
The ball milling medium is absolute ethyl alcohol, the ball milling frequency is 20-40Hz, and the ball milling time is 10-15 hours.
The second drying temperature is 70-90 ℃ and the drying time is 5-15 hours.
The activation temperature is 300-500 ℃ and the time is 1-3 hours.
The load applied to the physical pressing block is 500-700 megapascals, and the loading time is 5-10 minutes.
The second high temperature sintering includes: the block obtained after briquetting is respectively heated at 80 ℃, 100 ℃ and 150 ℃ for 20-40 minutes, then heated to 300 ℃ at the heating rate of 5-15 ℃/min, then heated to 600 ℃ at the heating rate of 0.5-1.5 ℃/min and kept for 1.5-2.5 hours, then heated to 1600 ℃ at the heating rate of 5-15 ℃/min and kept for 15-25 hours, and cooled to 300 ℃ at the cooling rate of 0.5-1.5 ℃/min after the heat preservation is completed, and then cooled to room temperature along with a furnace. This preferred mode is effective in preventing cracking in the resulting coated mass.
The X-ray diffraction measurement of the coated block prepared by the above embodiment shows that the main component of the prepared block material is m-YTAO as shown in the XRD curve of figure 2 4 And t-ZrO 2 。
The invention further provides the following preferred embodiments, each of which employs the following test methods:
anti-CMAS test of samples:
will CaO, mgO, al 2 O 3 、SiO 2 The powder comprises the following components in percentage by mole: mgO (MgO) 2 ：AlO 1.5 ：SiO 2 =33: 9:13:45 Mechanically mixing, heating at 1300 deg.C in a box-type resistance furnace for 8 hr, cooling, ball milling to obtain powder with particle size of about 30 μm, and mixing with CMAS at 10mg/cm 2 Is uniformly coated onThe prepared coated block surfaces with different components are then placed in a resistance furnace at 1250 ℃ for corrosion for 4 hours, then cooled along with the furnace, the sections of the corroded samples are made into metallographic samples, the corrosion areas of CMAS on the block are characterized by a Scanning Electron Microscope (SEM) with an energy spectrometer (EDS), and the penetration depth of the CMAS in the coating and the interface spheroidization phenomenon are compared.
Example 1
1.79g of tantalum pentachloride (TaCl) was weighed out separately 5 ) 1.92g of yttrium nitrate hexahydrate (Y (NO) 3 ) 3 ·6H 2 O) and 3.47g of zirconyl nitrate (ZrO (NO) 3 ) 2 ) Namely Ta of the prepared coating sample: y: zr atomic ratio is 2:2:6, preparing a base material;
TaCl to be weighed 5 Dissolving in absolute ethanol, and separating Y (NO 3 ) 3 ·6H 2 O and ZrO (NO) 3 ) 2 Respectively dissolving in distilled water, mixing the three solutions, and stirring for 0.5h by a magnetic stirrer to fully dissolve the solvent;
dripping the mixed solution into ammonia water with the pH value of 11 to obtain white gelatinous precipitate;
centrifuging the precipitate, washing with distilled water for 2 times, performing suction filtration by a vacuum device consisting of a sand core filter, a rubber tube and a conical flask, and drying at 80 ℃ for 48 hours to obtain precipitate powder;
placing the precipitated powder into a sintering furnace for high-temperature sintering, wherein the sintering temperature is 1600 ℃, and the sintering time is 10 hours;
the obtained powder is simply ground by an agate mortar, ball-milled for 24 hours at the frequency of 30Hz under the condition of taking absolute ethyl alcohol as a grinding medium, the slurry is dried for 10 hours at 80 ℃, activated for 2 hours at 400 ℃, and properly ground and dispersed by the agate mortar to obtain nano-scale powder;
1.5g of zirconium tantalum coating powder and yttrium oxide stabilized zirconia (7 YSZ) powder to be sintered are respectively weighed on an electronic balance, respectively poured into a columnar hollow graphite mold with the diameter of 12.5mm, then are pressed by a matched graphite pressing head, are loaded for 5 minutes under 600MPa by a static press, and then the taken sample is sintered at high temperature at 1600 ℃ to finally obtain two graphite powder with the size ofWherein the morphology of the resulting zirconium tantalum coated block sample is shown in FIG. 3;
respectively weighing 33.17g of calcium oxide (CaO), 6.46g of magnesium oxide (MgO) and 11.90g of (Al) 2 O 3 ) 48.47g of silicon oxide (SiO 2 ) Uniformly mixing the powder in an agate mortar, placing the powder in a box-type resistance furnace at 1300 ℃ for constant temperature heating for 8 hours, cooling the powder along with the furnace, and performing ball milling on the formed glassy CMAS to obtain powder with the granularity of about 30 mu m;
weighing two 4.906mg CMAS powder, respectively uniformly coating one round surface of the obtained zirconium tantalum coating block and one round surface of the obtained YSZ block, then placing the blocks in a high-temperature resistance furnace for corrosion experiment, wherein the corrosion temperature is 1250 ℃, and the corrosion time is 4 hours;
the corroded sample is prepared into a scanning electron microscope sample, the CMAS corrosion reaction layer thickness of the YSZ sample and the zirconium tantalum sample is compared by using a scanning electron microscope and an energy spectrometer, and the result is shown in figure 4, and compared with the YSZ coating, the zirconium tantalum coating can effectively reduce the CMAS reaction layer thickness, and the spheroidization phenomenon at the corrosion interface of the zirconium tantalum coating can be obviously reduced through an enlarged view of the corrosion interface (a small view part is an enlarged view of the corrosion interface part in a frame line), so that the zirconium tantalum coating has better CMAS corrosion resistance.
Example 2
1.43g of tantalum pentachloride (TaCl) was weighed out separately 5 ) 1.53g of yttrium nitrate hexahydrate (Y (NO) 3 ) 3 ·6H 2 O) and 0.46g of zirconyl nitrate (ZrO (NO) 3 ) 2 ) Namely Ta of the prepared coating sample: y: zr atomic ratios are 4:4:2;
the desired coating samples were prepared using the preparation method and corrosion parameters described in example 1 and CMAS corrosion experiments were performed. And (3) representing the corrosion interface of the YSZ sample and the zirconium tantalum sample after CMAS corrosion by using a scanning electron microscope (the result is shown in figure 5), wherein the YSZ corrosion interface is found to be seriously spheroidized, and the zirconium tantalum block corrosion interface has no obvious spheroidization phenomenon, which indicates that compared with the traditional YSZ coating, the zirconium tantalum coating has better stability after corrosion.
Example 3
The zirconium tantalum coating and the YSZ coating of the components described in the examples 1 and 2 are respectively prepared, and the samples before and after corrosion under the same corrosion parameters are respectively subjected to a Vickers indentation experiment, the load is 50N, the retention time is 15s, and the Vickers hardness of the sample is obtained. According to the calculation formula
Young's moduli of the three groups of specimens before and after corrosion were obtained, respectively. Wherein E is r Is equivalent elastic modulus, S is contact stiffness, A c Is the projection of the contact area between the pressure head and the sample, v and v i Poisson ratio of material and indenter, respectively, v in this case i ＝0.07。E i The Young's modulus of the indenter, E is the Young's modulus of the material.
According to the calculation formula
The fracture toughness before and after corrosion of the three groups of samples was obtained respectively. Where k is the fracture toughness of the sample and δ is the geometric constant, in this case δ=0.015; e is Young's modulus of the test specimen, H is hardness of the test specimen, P is loading load, and c is indentation crack length.
The mechanical property data of the zirconium tantalum coating and the YSZ coating obtained by the method before corrosion are shown in the following table 1, and the mechanical property after corrosion is shown in figure 2.
TABLE 1
It can be seen from the table that before corrosion, compared with the YSZ coating, the zirconium tantalum coating with two components has smaller Young's modulus, vickers hardness and larger fracture toughness, which indicates that the zirconium tantalum coating has better mechanical property compared with the YSZ coating and can meet the requirements of the thermal barrier coating; comparing the performance parameters of the corroded coating, the Young modulus and hardness of the zirconium tantalum coating with two components are still higher than those of the corroded YSZ coating, the fracture toughness is still lower than that of the corroded YSZ coating, and the variation before and after corrosion is smaller than that of the YSZ coating, as shown in the numerical values in brackets in Table 2:
TABLE 2
Note that: the values in brackets indicate the values of the parameters before and after corrosion
Indicating that CMAS corrosion has less impact on the mechanical properties of the zirconium tantalum coating than the YSZ coating, thereby indicating that the zirconium tantalum coating has higher corrosion resistance and stability than the YSZ coating.
The above examples are only preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the concept of the invention belong to the protection scope of the invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (6)
1. A preparation method of a zirconium-tantalum thermal barrier coating material is characterized by comprising the following steps:
TaCl is prepared according to the proportion requirement 5 、Y(NO 3 ) 3 ·6H 2 O、ZrO(NO 3 ) 2 Respectively dissolving to obtain corresponding raw material solutions;
mixing the obtained raw material solutions, adding the mixture into ammonia water, reacting to obtain colloidal precipitate, separating the colloidal precipitate, and performing first drying to obtain precipitate powder;
sintering the precipitated powder at a first high temperature of 1500-1700 ℃ for 10-15 hours to obtain first sintered powder;
ball milling is carried out on the first sintered powder, and the obtained ball milling powder is subjected to second drying and heating activation to obtain powder of the coating material;
wherein, the liquid crystal display device comprises a liquid crystal display device,
the proportioning requirements are as follows: the atomic ratio of Ta, Y and Zr in the component is 1:1:3, a step of;
the solvent of the raw material solution is selected from absolute ethyl alcohol and/or distilled water;
the temperature of the first drying is 70-90 ℃ and the time is 20-50 hours; the temperature of the second drying is 70-90 ℃ and the time is 5-15 hours;
the activation temperature is 300-500 ℃ and the activation time is 1-3 hours;
the obtained coating material contains m-YTaO 4 And t-ZrO 2 。
2. The method of manufacturing according to claim 1, further comprising: and carrying out static pressure molding on the powder of the coating material, and carrying out second high-temperature sintering on the molded body at 1500-1700 ℃ to obtain a block of the coating material.
3. The method of claim 2, wherein the second high temperature sintering process comprises: the molded body is heated to 300 ℃ at the temperature of 80 ℃ and 100 ℃ and 150 ℃ respectively for 20-40 minutes at the temperature rising rate of 5-15 ℃/min, then heated to 600 ℃ at the temperature rising rate of 0.5-1.5 ℃/min and kept for 1.5-2.5 hours, then heated to 1600 ℃ at the temperature rising rate of 5-15 ℃/min and kept for 15-25 hours, and cooled to 300 ℃ at the temperature reducing rate of 0.5-1.5 ℃/min after the heat preservation is completed, and then naturally cooled.
4. A method of preparation according to claim 3, wherein the shaping is carried out at a pressure of 500-700 mpa and/or for a time of 5-10 minutes.
5. The method according to claim 1, wherein the ball milling medium is absolute ethyl alcohol, the ball milling frequency is 20-40Hz, and the ball milling time is 10-15 hours.
6. The zirconium-tantalum thermal barrier coating material prepared by the preparation method according to any one of claims 1 to 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111104975.5A CN113773075B (en) | 2021-09-22 | 2021-09-22 | CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111104975.5A CN113773075B (en) | 2021-09-22 | 2021-09-22 | CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113773075A CN113773075A (en) | 2021-12-10 |
| CN113773075B true CN113773075B (en) | 2023-08-18 |
Family
ID=78852571
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111104975.5A Active CN113773075B (en) | 2021-09-22 | 2021-09-22 | CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113773075B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114835488A (en) * | 2022-04-22 | 2022-08-02 | 昆明理工大学 | Zirconia-based ceramic material without phase change and preparation method thereof |
| CN114804898A (en) * | 2022-04-22 | 2022-07-29 | 深圳清华大学研究院 | Multi-component co-doped zirconia thermal barrier coating material and preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234897A (en) * | 2008-03-03 | 2008-08-06 | 哈尔滨工业大学 | Method for preparing multi-component zirconium oxide based heat barrier oxide ceramic material |
| JP2010229471A (en) * | 2009-03-26 | 2010-10-14 | Mitsubishi Heavy Ind Ltd | Material for thermal barrier coating, thermal barrier coating, turbine member, and gas turbine |
| CN102245810A (en) * | 2008-12-15 | 2011-11-16 | 阿尔斯通技术有限公司 | Thermal barrier coating system, components coated therewith and method for applying a thermal barrier coating system to components |
| CN103145430A (en) * | 2013-03-22 | 2013-06-12 | 西北有色金属研究院 | Multi-element stabilized zirconia fused salt corrosion-resisting thermal barrier coating material |
| CN106588042A (en) * | 2016-11-18 | 2017-04-26 | 北京理工大学 | Ternary rare earth doped YSZ thermal barrier coating material and preparation method thereof |
| CN111850454A (en) * | 2020-07-30 | 2020-10-30 | 江苏大学 | CMAS erosion resistant thermal barrier coating and preparation method thereof |
| CN111908921A (en) * | 2020-08-28 | 2020-11-10 | 昆明理工大学 | Rare earth tantalate (RE3TaO7) thermal barrier coating and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013068315A1 (en) * | 2011-11-10 | 2013-05-16 | Alstom Technology Ltd | High temperature thermal barrier coating |
-
2021
- 2021-09-22 CN CN202111104975.5A patent/CN113773075B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234897A (en) * | 2008-03-03 | 2008-08-06 | 哈尔滨工业大学 | Method for preparing multi-component zirconium oxide based heat barrier oxide ceramic material |
| CN102245810A (en) * | 2008-12-15 | 2011-11-16 | 阿尔斯通技术有限公司 | Thermal barrier coating system, components coated therewith and method for applying a thermal barrier coating system to components |
| JP2010229471A (en) * | 2009-03-26 | 2010-10-14 | Mitsubishi Heavy Ind Ltd | Material for thermal barrier coating, thermal barrier coating, turbine member, and gas turbine |
| CN103145430A (en) * | 2013-03-22 | 2013-06-12 | 西北有色金属研究院 | Multi-element stabilized zirconia fused salt corrosion-resisting thermal barrier coating material |
| CN106588042A (en) * | 2016-11-18 | 2017-04-26 | 北京理工大学 | Ternary rare earth doped YSZ thermal barrier coating material and preparation method thereof |
| CN111850454A (en) * | 2020-07-30 | 2020-10-30 | 江苏大学 | CMAS erosion resistant thermal barrier coating and preparation method thereof |
| CN111908921A (en) * | 2020-08-28 | 2020-11-10 | 昆明理工大学 | Rare earth tantalate (RE3TaO7) thermal barrier coating and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Y0.5-x/2Ta0.5-x/2ZrxO2新型热障涂层材料抗CMAS腐蚀成分优化研究;罗成;《中国稀土学会2020学术年会暨江西(赣州)稀土资源绿色开发与高效利用大会摘要集》;20201031;第343页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113773075A (en) | 2021-12-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113773075B (en) | CMAS erosion resistant zirconium-tantalum thermal barrier coating material and preparation method thereof | |
| Maji et al. | Microstructure and mechanical properties of alumina toughened zirconia (ATZ) | |
| US5447894A (en) | Sintered ceramic article formed mainly of alumina | |
| Dressler et al. | Model experiments concerning abnormal grain growth in silicon nitride | |
| JP2005026593A (en) | Ceramic product, corrosion-resistant member, and method of manufacturing ceramic product | |
| Hoffmann | Analysis of microstructural development and mechanical properties of Si3N4 ceramics | |
| US4764491A (en) | Low temperature sintering of yttria stabilized zirconia with lanthana borate additions | |
| CN101218188B (en) | Sintered yttria, anticorrosion member and process for producing the same | |
| CN110105057A (en) | Ceramic arm and preparation method thereof, vacuum suction machinery hand and wafer conveying device | |
| Li et al. | Fabrication of calcium hexaluminate‐based porous ceramic with microsilica addition | |
| JPS61101462A (en) | Zirconia ceramic | |
| Zhu et al. | Texture development in Si3N4 ceramics by magnetic field alignment during slip casting | |
| Zhao et al. | Influence of yttrium oxide addition and sintering temperature on properties of alumina‐based ceramic cores | |
| CN112723412B (en) | Multiphase rare earth zirconate material and preparation method and application thereof | |
| CN112110740B (en) | Method for preparing aluminum oxide-based composite biological ceramic material through in-situ reaction and product prepared by method | |
| Zhang et al. | Mechanical reinforcement of 3D printed cordierite-zirconia composites | |
| Wei et al. | Phase transformation and grain coarsening of zirconia/mullite composites | |
| Herrmann et al. | Hydrothermal corrosion of zirconia-toughened alumina (ZTA) at 200 C | |
| Wu et al. | ZrO2‐doped YTaO4 as potential CMAS‐resistant materials for thermal barrier coatings application | |
| CN115057704A (en) | Rare earth block ceramic material for resisting sediment corrosion in sand environment and preparation method and application thereof | |
| CN109678504B (en) | High-temperature divalent magnesium ion doped yttrium tantalate ceramic and preparation method thereof | |
| CN102503418B (en) | Low-temperature liquid-phase sintered La2Zr2O7 ceramics and sintering method thereof | |
| Brito-Chaparro et al. | Using high-purity MgO nanopowder as a stabilizer in two different particle size monoclinic ZrO2: Its influence on the fracture toughness | |
| JP2001526175A (en) | Dense refractories with improved heat shock resistance | |
| JP3148559B2 (en) | Ceramic fiber reinforced turbine blade and method of manufacturing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |