CN113816751B - Tetragonal phase high-entropy thermal barrier coating material and preparation method thereof - Google Patents
Tetragonal phase high-entropy thermal barrier coating material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a tetragonal phase high-entropy thermal barrier coating material which is prepared from ZrO 2 、Y 2 O 3 、M 2 O 3 、Ta 2 O 5 And Nb 2 O 5 Oxide powder of Zr as constituent 1‑4x Y x M x Ta x Nb x O 2 Wherein, 0<x<0.25, M is a trivalent rare earth element. The invention also relates to a preparation method of the tetragonal phase high-entropy thermal barrier coating material, which comprises the steps of removing adsorbed water and impurities in each oxide powder by calcination; carrying out high-energy ball milling; separating, washing and drying the ball material to obtain mixed powder; and pressing the mixture into a ceramic blank by using a ceramic tablet press, and heating to obtain the high-entropy ceramic block material. According to the tetragonal phase high-entropy thermal barrier coating material, excellent thermodynamic properties including reduction of thermal conductivity, increase of thermal expansion coefficient, enhancement of fracture toughness, good high-temperature stability, excellent CMAS corrosion resistance and the like are provided through multi-component high-entropy transformation, and the tetragonal phase high-entropy thermal barrier coating material has the potential of serving at higher gas temperature.
Description
Technical Field
The invention relates to a thermal barrier coating, in particular to a tetragonal high-entropy thermal barrier coating material and a preparation method thereof.
Background
Thermal Barrier Coatings (Thermal Barrier Coatings) are used to protect alloy blades of high pressure turbine components in ground gas turbines and aircraft engines from corrosion and oxidation by high temperature combustion gases, increasing turbine inlet temperatures, and thereby greatly improving the operating efficiency of gas turbines and aircraft engines.
The most widely used thermal barrier coating material at present is 7-8 wt% yttria stabilized zirconia (7-8 YSZ). In order to pursue higher working efficiency of the gas turbine, the gas using temperature of the next generation of the gas turbine must exceed 1500 ℃, and is higher than the using range of the current 7-8 YSZ thermal barrier coating. The known thermal barrier coating material has the defects of poor high-temperature phase stability, low thermal conductivity, poor CMAS resistance and the like.
Disclosure of Invention
In order to solve the problems of poor high-temperature phase stability and the like of the known thermal barrier coating material in the prior art, the invention provides a tetragonal phase high-entropy thermal barrier coating material and a preparation method thereof.
The tetragonal phase high-entropy thermal barrier coating material consists of ZrO 2 、Y 2 O 3 、M 2 O 3 、Ta 2 O 5 And Nb 2 O 5 Oxide powder of Zr as constituent 1-4x Y x M x Ta x Nb x O 2 Wherein, 0<x<0.25, M is a trivalent rare earth element.
Preferably, M is Yb, La or Eu.
Preferably, 0.088<x<0.2. In a preferred embodiment, the constituent elements of the tetragonal phase high entropy thermal barrier coating materialIs Zr 0.2 Y 0.2 Yb 0.2 Ta 0.2 Nb 0.2 O 2 、Zr 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 、Zr 0.524 Y 0.119 Yb 0.119 Ta 0.119 Nb 0.119 O 2 、Zr 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 。
Preferably, ZrO 2 (zirconium oxide) Y 2 O 3 (Yttrium oxide), M 2 O 3 (rare earth oxide), Ta 2 O 5 (tantalum oxide) and Nb 2 O 5 The purity of the oxide powder of (niobium oxide) is more than or equal to 99.5 percent.
The preparation method of the tetragonal phase high-entropy thermal barrier coating material comprises the following steps: s1, according to component Zr 1-4x Y x M x Ta x Nb x O 2 ZrO is respectively weighed according to atom percentage of each cation 2 、Y 2 O 3 、M 2 O 3 、Ta 2 O 5 、Nb 2 O 5 The oxide powder is respectively and gradually heated to 900-1100 ℃ and then is calcined and cooled, and the adsorbed water and impurities in the oxide powder are removed; s2, pouring the calcined oxide powder into a high-energy ball milling tank, adding a first organic solvent and milling balls, and performing high-energy ball milling, wherein the ball-to-material ratio is 5-10: 1; s3, performing ball material separation on the suspension after the high-energy ball milling, washing by adopting a second organic solvent, drying, grinding and sieving to obtain mixed powder with the particle size of 1-10 microns; s4, pressing the obtained mixed powder into a ceramic blank by using a ceramic tablet press under the pressure of 150-300 MPa, then gradually heating to 1500-1700 ℃, and then cooling to obtain the high-entropy ceramic block material.
Preferably, in the step S1, the oxide powders are respectively placed in different crucibles, and are placed in a box-type muffle furnace to be insulated at 1100 ℃ for 1-3 h, wherein the heating rate and the cooling rate are controlled to be 2-10 ℃/min. In a preferred embodiment, the crucible is an alumina crucible. In a preferred embodiment, the sample is placed in a box muffle furnace and incubated at 1000 ℃ for 2 h. In a preferred embodiment, the rate of temperature rise and the rate of temperature fall are both 5 to 8 ℃/min. In a preferred embodiment, the box muffle is a high temperature box muffle model L1700, manufactured by Shanghai Kejing, Inc.
Preferably, in the step S2, the first organic solvent is isopropyl alcohol. More preferably, 80-120ml of isopropanol are added. In a preferred embodiment, 90-110ml of isopropanol are added. In a preferred embodiment, 100ml of isopropanol are added. It should be understood that the first organic solvent may also be other solvents, such as ethanol, distilled water, etc., which function to adsorb on the surface of each oxide powder, reduce surface activity, and impair the ability of the powder to agglomerate.
Preferably, in the step S2, the grinding balls are zirconia grinding balls. It should be understood that the use of zirconia balls does not introduce other impurities because the matrix material includes zirconia. More preferably, the diameter of the grinding ball is 0.3-0.5 mm. In a preferred embodiment, the grinding balls have a diameter of 0.4 mm. In a preferred embodiment, the ball to feed ratio is 8: 1. In a preferred embodiment, the high energy ball mill is a model 01-HDDM 750cc high energy ball mill and zirconia liner, manufactured by Union Process Inc., USA.
Preferably, in the step S2, the ball milling rotation speed is 2000 to 3000r/min, and the ball milling time is 6 to 12 hours. In a preferred embodiment, the ball milling speed is 2100r/min to 2700 r/min. In a preferred embodiment, the ball milling speed is 2500 r/min. In a preferred embodiment, the ball milling time is 8 h.
Preferably, in the step S3, the second organic solvent is absolute ethanol or isopropanol. In a preferred embodiment, washing is carried out 4-6 times by absolute ethyl alcohol or isopropanol. In a preferred embodiment, the purity of the absolute ethanol and isopropanol is greater than or equal to 99.5%.
Preferably, in the step S3, the mixed suspension obtained after washing is dried in an electrothermal blowing dry box at 80-120 ℃ for 24-48 h, and then ground and sieved. In a preferred embodiment, the mixture is dried in an electrothermal blowing dry box at 90-100 ℃ for 40-48h, and then ground and sieved to obtain mixed powder with the particle size of about 3-6 microns. In a preferred embodiment, the milling screens produce a blended powder having a particle size of about 4 microns.
Preferably, in the step S4, the obtained mixed powder is pressed into a ceramic green body by using a ceramic pressing machine under a pressure of 200 MPa. In a preferred embodiment, the ceramic tablet press is a YLJ-30T-LD type tablet press manufactured by Hefeiki Crystal Co., Ltd.
Preferably, in the step S4, the ceramic green body is placed into a box-type muffle furnace to be heated from room temperature to 1500-1700 ℃ at a speed of 2-10 ℃/min, and is kept for 12-40 h, and is cooled from 1600 ℃ to 1100 ℃ at a speed of 30-50 ℃/min, and is cooled from 1100 ℃ to room temperature at a speed of 5-10 ℃/min, so as to obtain the high-entropy ceramic block material. In a preferred embodiment, the heating is carried out in a box muffle furnace to 1600 ℃ for 20 h. In a preferred embodiment, the temperature rising rate is controlled to be 5 ℃/min, the temperature reducing rate is controlled to be 33-44 ℃/min from 1600 ℃ to 1100 ℃, and the temperature is controlled to be 10 ℃/min from 1100 ℃ to room temperature. In a preferred embodiment, the box muffle is a high temperature box muffle of type L1700 manufactured by Shanghai Kejing, Inc.
According to the tetragonal high-entropy thermal barrier coating material, the entropy value of the original system is increased through multi-element co-doping (including all trivalent elements, pentavalent elements and various rare earth elements; such as yttrium, ytterbium, tantalum, niobium and the like), and the phase composition, the grain size, the thermal properties (including thermal conductivity, thermal expansion coefficient and the like) and the mechanical properties (including hardness, Young modulus, fracture toughness and the like) of the obtained tetragonal high-entropy thermal barrier coating material can be regulated and controlled. On the one hand, the high-entropy oxide Zr of single or double tetragonal phase is prepared 1-4x Y x M x Ta x Nb x O 2 Stabilizing a tetragonal phase structure which can only exist at high temperature to room temperature, so that even if a little component deviation occurs in the thermal spraying process, the phase component of the whole thermal barrier coating can be ensured not to deviate; on the other hand, the high entropy of the multi-component provides excellent thermodynamic properties, including the reduction of thermal conductivity (1.16-1.84W mK) -1 900 ℃ C.), and an increased thermal expansion coefficient (9.01 to 11.3X 10) -6 K -1 1000 ℃ C.), and enhanced fracture toughness (1.56-4.59 MPa m) 1/2 ) Good high temperatureStability (no phase change occurs after heat treatment for 100 hours at 1600 ℃), excellent CMAS corrosion resistance (corrosion rate of 2.9 mu m/h), and the like, and has the potential of serving at higher fuel gas temperature (1600 ℃).
Drawings
FIG. 1 is Zr prepared according to example 2 of the present invention 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 An XRD pattern of (a);
FIG. 2 is Zr prepared according to example 2 of the present invention 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 BSE picture of (c);
FIG. 3 is Zr prepared according to example 2 of the present invention 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 Coefficient of thermal expansion of (a);
FIG. 4 shows Zr prepared according to example 4 of the present invention 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 An XRD pattern of (a);
FIG. 5 is Zr prepared according to example 4 of the present invention 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 BSE picture of (c);
FIG. 6 shows Zr prepared according to example 4 of the present invention 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 The coefficient of thermal expansion of (a).
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
Multicomponent Zr designed according to high entropy 1-4x Y x M x Ta x Nb x O 2 Weighing a certain amount of oxide powder (wherein x is 0.2, and the component is Zr) 0.2 Y 0.2 Yb 0.2 Ta 0.2 Nb 0.2 O 2 ) Comprising ZrO of 2 、Y 2 O 3 、Yb 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And respectively placing the oxide powder into different alumina crucibles, placing the alumina crucibles into a box-type muffle furnace, and keeping the temperature for 2 hours at 1000 ℃, wherein the heating rate and the cooling rate are controlled to be 5 ℃/min, so as to remove adsorbed water and impurities in the original powder.
And pouring various calcined oxide powders into a high-energy ball milling tank, adding a certain amount of isopropanol (100ml) and zirconia milling balls (0.3mm, the ball-to-material ratio is 10:1), and performing high-energy ball milling at the ball milling rotation speed of 2500/min for 12 h.
And (3) ball material separation is carried out on the suspension liquid after the high-energy ball milling is finished, absolute ethyl alcohol is adopted for washing for 6 times, the obtained mixed suspension liquid is placed in an electrothermal blowing drying oven at 100 ℃ for drying for 48 hours, and then grinding and sieving are carried out, so that mixed powder with the particle size of about 3 microns can be obtained.
Pressing the obtained mixed powder into a ceramic blank body with a certain size by using a ceramic tablet press under the pressure of 300MPa, then placing the ceramic blank body into a box-type muffle furnace, keeping the temperature for 20 hours at 1600 ℃, controlling the heating rate to be 5 ℃/min, the cooling rate to be 40 ℃/min from 1600 ℃ to 1100 ℃, and the cooling rate to be 10 ℃/min from 1100 ℃ to room temperature, and obtaining the final high-entropy Zr 0.2 Y 0.2 Yb 0.2 Ta 0.2 Nb 0.2 O 2 A ceramic bulk material. The thermal conductivity of the obtained high-entropy ceramic is 1.23W mK -1 (900 ℃ C.); coefficient of thermal expansion of 10.3X 10 -6 K -1 (1000 ℃ C.); the fracture toughness is 1.96MPa m 1/2 (ii) a The CMAS corrosion rate is 2.2 mu m/h.
The purity of the oxidized powder zirconium oxide, yttrium oxide, rare earth oxide, tantalum oxide and niobium oxide is more than or equal to 99.5 percent.
The box-type muffle furnace is an L1700 type high-temperature box-type muffle furnace produced by Shanghai Kejing company Limited.
The high energy ball mill is a 01-HDDM 750cc high energy ball mill and a zirconia liner manufactured by Union Process Inc. of America.
The purity of the absolute ethyl alcohol and the isopropanol is more than or equal to 99.5 percent.
The ceramic tablet press is a YLJ-30T-LD type tablet press produced by Hefei Kejing Co.
Example 2
Multicomponent Zr designed according to high entropy 1-4x Y x M x Ta x Nb x O 2 Weighing a certain amount of oxide powder (wherein x is 0.179, and the component is Zr) 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 ) Comprising ZrO 2 、Y 2 O 3 、Yb 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And respectively placing the oxide powder into different alumina crucibles, placing the alumina crucibles into a box-type muffle furnace, and keeping the temperature for 1h at 1000 ℃, wherein the heating rate and the cooling rate are controlled to be 10 ℃/min, so as to remove adsorbed water and impurities in the original powder.
Pouring various calcined oxide powders into a high-energy ball milling tank, adding a certain amount of isopropanol (120ml) and zirconia grinding balls (0.4mm, the ball-material ratio is 10:1), and carrying out high-energy ball milling at the ball milling rotation speed of 2100r/min for 12 h.
And (3) ball material separation is carried out on the suspension liquid after the high-energy ball milling is finished, isopropanol is adopted for washing for 6 times, the obtained mixed suspension liquid is placed in an electrothermal blowing drying oven at the temperature of 120 ℃ for drying for 48 hours, and then grinding and sieving are carried out, so that mixed powder with the particle size of about 4 micrometers can be obtained.
Pressing the obtained mixed powder into a ceramic blank body with a certain size by using a ceramic tablet press under the pressure of 300MPa, then putting the ceramic blank body into a box-type muffle furnace, and keeping the temperature for 20h at 1600 ℃ and controlling the heating rate to be 5 ℃/min, the cooling rate to be 33 ℃/min from 1600 ℃ to 1100 ℃ and the cooling rate to be 10 ℃/min from 1100 ℃ to room temperature to obtain the final high-entropy Zr 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 A ceramic bulk material. The thermal conductivity of the obtained high-entropy ceramic is 1.44W mK -1 (900 ℃); the fracture toughness is 2.10MPa m 1/2 (ii) a The CMAS corrosion rate is 2.4 mu m/h.
FIG. 1 shows Zr prepared 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 XRD patterns of high entropy oxidesSpectrum, from this, it is clear that Zr 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 High entropy oxide as high temperature tetragonal phase ABO 4 The structure (wherein A is rare earth element, B is Ta/Nb), due to the lattice distortion generated by multicomponent doping, the XRD peak position deviates rightwards from the PDF NO.50-0846 as a whole, but the basic peak position is matched with the XRD peak position.
FIG. 2 shows Zr prepared 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 BSE pictures of the high-entropy oxide show that the grain size is uniform and presents a tetragonal crystal morphology, the crystal grain size is about 10 mu m without precipitation of other phases, and basically, the structure is a single tetragonal phase structure.
FIG. 3 shows Zr produced 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 The thermal expansion coefficient of the high-entropy oxide was found to be 9.93X 10 at 1000 ℃ -6 K -1 The thermal barrier coefficient (10.5 multiplied by 10) of the current commercial thermal barrier coating material YSZ is close to -6 K -1 ,1000℃)。
The purity of the oxidized powder zirconium oxide, yttrium oxide, rare earth oxide, tantalum oxide and niobium oxide is more than or equal to 99.5 percent.
The box-type muffle furnace is an L1700 type high-temperature box-type muffle furnace produced by Shanghai Kejing company Limited.
The high energy ball mill is a 01-HDDM 750cc high energy ball mill and a zirconia liner manufactured by Union Process Inc. of America.
The purity of the absolute ethyl alcohol and the isopropanol is more than or equal to 99.5 percent.
The ceramic tablet press is a YLJ-30T-LD type tablet press produced by Hefei Kejing Co.
Example 3
Multicomponent Zr designed according to high entropy 1-4x Y x M x Ta x Nb x O 2 Weighing a certain amount of oxide powder (wherein x is 0.119, and the component is Zr) 0.524 Y 0.119 Yb 0.119 Ta 0.119 Nb 0.119 O 2 ) Comprising ZrO of 2 、Y 2 O 3 、Yb 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And respectively placing the oxide powder into different alumina crucibles, placing the alumina crucibles into a box-type muffle furnace, and keeping the temperature for 3 hours at 1000 ℃, wherein the heating rate and the cooling rate are controlled to be 8 ℃/min, so as to remove adsorbed water and impurities in the original powder.
And pouring various calcined oxide powders into a high-energy ball milling tank, adding a certain amount of isopropanol (90ml) and zirconia milling balls (0.3mm, the ball-to-material ratio is 8:1), and performing high-energy ball milling at the ball milling rotation speed of 2700r/min for 8 hours.
And (3) ball material separation is carried out on the suspension liquid after the high-energy ball milling is finished, isopropanol is adopted for washing for 5 times, the obtained mixed suspension liquid is placed in an electrothermal blowing drying oven at 90 ℃ for drying for 40 hours, and then grinding and sieving are carried out, so that mixed powder with the particle size of about 6 microns can be obtained.
Pressing the obtained mixed powder into a ceramic blank body with a certain size by using a ceramic tablet press under the pressure of 200MPa, then placing the ceramic blank body into a box-type muffle furnace, and keeping the temperature for 30 hours at 1600 ℃, wherein the heating rate is controlled to be 8 ℃/min, the cooling rate is controlled to be 44 ℃/min from 1600 ℃ to 1100 ℃, and the cooling rate is controlled to be 5 ℃/min from 1100 ℃ to room temperature, so as to obtain the final high-entropy Zr 0.524 Y 0.119 Yb 0.119 Ta 0.119 Nb 0.119 O 2 A ceramic bulk material. The thermal conductivity of the obtained high-entropy ceramic is 1.20W mK -1 (900 ℃ C.); coefficient of thermal expansion of 11.0X 10 -6 K -1 (1000 ℃ C.); the fracture toughness is 4.51MPa m 1/2 (ii) a The CMAS corrosion rate is 2.5 mu m/h.
The purity of the oxidized powder zirconium oxide, yttrium oxide, rare earth oxide, tantalum oxide and niobium oxide is more than or equal to 99.5 percent.
The box-type muffle furnace is an L1700 type high-temperature box-type muffle furnace produced by Shanghai Kejing company Limited.
The high energy ball mill is a 01-HDDM 750cc high energy ball mill and a zirconia liner manufactured by Union Process Inc. of America.
The purity of the absolute ethyl alcohol and the isopropanol is more than or equal to 99.5 percent.
The ceramic tablet press is a YLJ-30T-LD type tablet press produced by Hefei Kejing Co.
Example 4
Multicomponent Zr designed according to high entropy 1-4x Y x M x Ta x Nb x O 2 Weighing a certain amount of oxide powder (wherein x is 0.088, and the component is Zr) 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 ) Comprising ZrO of 2 、Y 2 O 3 、Yb 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And respectively placing the oxide powder into different alumina crucibles, placing the alumina crucibles into a box-type muffle furnace, and keeping the temperature for 1h at 1000 ℃, wherein the heating rate and the cooling rate are controlled to be 5 ℃/min, so as to remove adsorbed water and impurities in the original powder.
Pouring various calcined oxide powders into a high-energy ball milling tank, adding a certain amount of isopropanol (110ml) and zirconia grinding balls (0.4mm, the ball-material ratio is 10:1), and carrying out high-energy ball milling at the ball milling rotation speed of 2100r/min for 12 h.
And (3) performing ball material separation on the suspension after the high-energy ball milling, washing for 6 times by using isopropanol, drying the obtained mixed suspension in an electrothermal blowing drying oven at the temperature of 120 ℃ for 48 hours, and then grinding and sieving to obtain mixed powder with the particle size of about 3 micrometers.
Pressing the obtained mixed powder into a ceramic blank body with a certain size by using a ceramic tablet press under the pressure of 300MPa, then putting the ceramic blank body into a box-type muffle furnace, and keeping the temperature for 20h at 1600 ℃ with the temperature rising rate of 5 ℃/min, the temperature lowering rate of 30 ℃/min from 1600 ℃ to 1100 ℃ and the temperature from 1100 ℃ to room temperature of 10 ℃/min to obtain the final high-entropy Zr 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 A ceramic bulk material. The thermal conductivity of the obtained high-entropy ceramic is 1.32W mK -1 (900 ℃ C.); the fracture toughness is 2.42MPa m 1/2 (ii) a The CMAS corrosion rate is 2.3 mu m/h.
FIG. 4 shows Zr prepared 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 XRD pattern of high entropy oxide from which it is known that Zr 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 The high-entropy oxide is of a high-temperature tetragonal phase ZYTO structure, has good crystallinity, and the XRD peak position of the high-entropy oxide is identical with that of PDF NO. 43-0308.
FIG. 5 shows Zr prepared 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 BSE pictures of the high-entropy oxide show that the grain size is uniform and presents a tetragonal crystal morphology, the crystal grain size is about 16 mu m without precipitation of other phases, and basically, the structure is a single tetragonal phase structure.
FIG. 6 shows Zr produced 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 The thermal expansion coefficient of the high-entropy oxide was found to be 10.13X 10 at 1000 ℃ respectively -6 K -1 The thermal barrier coefficient (10.5 multiplied by 10) of the current commercial thermal barrier coating material YSZ is close to -6 K -1 ,1000℃)。
The purity of the oxidized powder zirconium oxide, yttrium oxide, rare earth oxide, tantalum oxide and niobium oxide is more than or equal to 99.5%.
The box-type muffle furnace is an L1700 type high-temperature box-type muffle furnace produced by Shanghai Kejing company Limited.
The high energy ball mill is a 01-HDDM 750cc high energy ball mill and a zirconia liner manufactured by Union Process Inc. of America.
The purity of the absolute ethyl alcohol and the isopropanol is more than or equal to 99.5 percent.
The ceramic tablet press is a YLJ-30T-LD type tablet press produced by Hefei Kejing Co.
Example 5
Multicomponent Zr designed according to high entropy 1-4x Y x M x Ta x Nb x O 2 In which the atom percentage of each cation is weighedEach oxide powder (wherein x is 0.2, and the constituent is Zr) 0.2 Y 0.2 Eu 0.2 Ta 0.2 Nb 0.2 O 2 ) Comprising ZrO 2 、Y 2 O 3 、Eu 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And respectively placing the oxide powder into different alumina crucibles, placing the alumina crucibles into a box-type muffle furnace, and keeping the temperature for 1h at 1000 ℃, wherein the heating rate and the cooling rate are controlled to be 5 ℃/min, so as to remove adsorbed water and impurities in the original powder.
Pouring various calcined oxide powders into a high-energy ball milling tank, adding a certain amount of isopropanol (110ml) and zirconia grinding balls (0.4mm, the ball-material ratio is 10:1), and carrying out high-energy ball milling at the ball milling rotation speed of 2100r/min for 12 h.
And (3) performing ball material separation on the suspension after the high-energy ball milling, washing for 6 times by using isopropanol, drying the obtained mixed suspension in an electrothermal blowing drying oven at the temperature of 120 ℃ for 48 hours, and then grinding and sieving to obtain mixed powder with the particle size of about 3 micrometers.
Pressing the obtained mixed powder into a ceramic blank body with a certain size by using a ceramic tablet press under the pressure of 300MPa, then putting the ceramic blank body into a box-type muffle furnace, and keeping the temperature for 20h at 1600 ℃ with the temperature rising rate of 5 ℃/min, the temperature lowering rate of 30 ℃/min from 1600 ℃ to 1100 ℃ and the temperature from 1100 ℃ to room temperature of 10 ℃/min to obtain the final high-entropy Zr 0.2 Y 0.2 Eu 0.2 Ta 0.2 Nb 0.2 O 2 A ceramic bulk material. The thermal conductivity of the obtained high-entropy ceramic is 1.19W mK -1 (900 ℃ C.); coefficient of thermal expansion of 9.3X 10 - 6 K -1 (1000 ℃ C.); the fracture toughness is 1.86MPa m 1/2 (ii) a The CMAS corrosion rate is 1.9 mu m/h.
The purity of the oxidized powder zirconium oxide, yttrium oxide, rare earth oxide, tantalum oxide and niobium oxide is more than or equal to 99.5%.
The box-type muffle furnace is an L1700 type high-temperature box-type muffle furnace produced by Shanghai Kejing company Limited.
The high energy ball mill is a 01-HDDM 750cc high energy ball mill and a zirconia liner manufactured by Union Process Inc. of America.
The purity of the absolute ethyl alcohol and the isopropanol is more than or equal to 99.5 percent.
The ceramic tablet press is a YLJ-30T-LD type tablet press produced by Hefei Kejing Co.
Comparative example 1
Multicomponent Zr designed according to high entropy 1-4x Y x M x Ta x Nb x O 2 Weighing a certain amount of oxide powder (wherein x is 0.088, and the component is Zr) 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 ) Comprising ZrO 2 、Y 2 O 3 、Yb 2 O 3 、Ta 2 O 5 、Nb 2 O 5 And respectively placing the oxide powder into different alumina crucibles, placing the alumina crucibles into a box-type muffle furnace, and keeping the temperature for 1h at 1000 ℃, wherein the heating rate and the cooling rate are controlled to be 5 ℃/min, so as to remove adsorbed water and impurities in the original powder.
Pouring various calcined oxide powders into a high-energy ball milling tank, adding a certain amount of isopropanol (110ml) and zirconia grinding balls (0.4mm, the ball-material ratio is 12:1), and carrying out high-energy ball milling at the ball milling rotation speed of 2100r/min for 12 h.
And (3) ball material separation is carried out on the suspension liquid after the high-energy ball milling is finished, isopropanol is adopted for washing for 6 times, the obtained mixed suspension liquid is placed in an electrothermal blowing drying oven at 120 ℃ for drying for 48 hours, and then grinding and sieving are carried out, so that mixed powder with the particle size of about 15 micrometers can be obtained.
Pressing the obtained mixed powder into a ceramic blank body with a certain size by using a ceramic tablet press under the pressure of 400MPa, then putting the ceramic blank body into a box-type muffle furnace, and keeping the temperature for 20h at 1600 ℃ with the temperature rising rate of 5 ℃/min, the temperature lowering rate of 30 ℃/min from 1600 ℃ to 1100 ℃ and the temperature from 1100 ℃ to room temperature of 10 ℃/min to obtain the final high-entropy Zr 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 A ceramic bulk material. The thermal conductivity of the obtained high-entropy ceramic is 1.63W mK -1 (900 ℃ C.); coefficient of thermal expansion of 8.3X 10 -6 K -1 (1000 ℃ C.); the fracture toughness is 1.76MPa m 1/2 (ii) a The CMAS corrosion rate is 2.9 mu m/h.
The purity of the oxidized powder zirconium oxide, yttrium oxide, rare earth oxide, tantalum oxide and niobium oxide is more than or equal to 99.5 percent.
The box-type muffle furnace is an L1700 type high-temperature box-type muffle furnace produced by Shanghai Kejing company Limited.
The high energy ball mill is a 01-HDDM 750cc high energy ball mill and a zirconia liner manufactured by Union Process Inc. of America.
The purity of the absolute ethyl alcohol and the isopropanol is more than or equal to 99.5 percent.
The ceramic tablet press is a YLJ-30T-LD type tablet press produced by Hefei Kejing Co.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and various modifications may be made to the above-described embodiment of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (9)
1. A tetragonal phase high entropy thermal barrier coating material is characterized in that the tetragonal phase high entropy thermal barrier coating material is composed of ZrO 2 、Y 2 O 3 、M 2 O 3 、Ta 2 O 5 And Nb 2 O 5 Oxide powder of Zr as constituent 1-4x Y x M x Ta x Nb x O 2 Wherein 0 is<x<0.25, M is Yb, La or Eu.
2. A tetragonal phase high entropy thermal barrier coating material as claimed in claim 1 wherein 0.088< x < 0.2.
3. A tetragonal phase high entropy thermal barrier coating material as claimed in claim 1, characterized by the components of the tetragonal phase high entropy thermal barrier coating materialIs Zr 0.2 Y 0.2 Yb 0.2 Ta 0.2 Nb 0.2 O 2 、Zr 0.284 Y 0.179 Yb 0.179 Ta 0.179 Nb 0.179 O 2 、Zr 0.524 Y 0.119 Yb 0.11 9 Ta 0.119 Nb 0.119 O 2 、Zr 0.648 Y 0.088 Yb 0.088 Ta 0.088 Nb 0.088 O 2 。
4. A method of producing a tetragonal high entropy thermal barrier coating material according to any one of claims 1-3, characterized in that the method comprises the steps of:
s1, according to component Zr 1-4x Y x M x Ta x Nb x O 2 ZrO is respectively weighed according to atom percentage of each cation 2 、Y 2 O 3 、M 2 O 3 、Ta 2 O 5 、Nb 2 O 5 The oxide powder is respectively and gradually heated to 900-1100 ℃ and then is calcined and cooled, and the adsorbed water and impurities in the oxide powder are removed;
s2, pouring the calcined oxide powder into a high-energy ball milling tank, adding a first organic solvent and milling balls, and performing high-energy ball milling, wherein the ball-to-material ratio is 5-10: 1;
s3, performing ball material separation on the suspension after the high-energy ball milling, washing by adopting a second organic solvent, drying, grinding and sieving to obtain mixed powder with the particle size of 1-10 microns;
s4, pressing the obtained mixed powder into a ceramic blank by using a ceramic tablet press under the pressure of 150-300 MPa, then gradually heating to 1500-1700 ℃, and then cooling to obtain the high-entropy ceramic block material.
5. The method as claimed in claim 4, wherein in step S1, the oxide powders are placed in different crucibles, and placed in a box-type muffle furnace to be maintained at 1100 ℃ for 1-3 h, wherein the temperature rising rate and the temperature lowering rate are both controlled to be 2-10 ℃/min.
6. The preparation method according to claim 4, wherein in the step S2, the ball milling rotation speed is 2000-3000 r/min, and the ball milling time is 6-12 h.
7. The production method according to claim 4, wherein in the step S2, the grinding balls are zirconia grinding balls.
8. The preparation method according to claim 4, wherein in the step S3, the mixed suspension obtained after washing is dried in an electrothermal blowing dry box at 80-120 ℃ for 24-48 h, ground and sieved.
9. The preparation method according to claim 4, wherein in the step S4, the ceramic green body is placed in a box-type muffle furnace to be heated from room temperature to 1500-1700 ℃ at a speed of 2-10 ℃/min, and is kept for 12-40 h, and is cooled from 1600 ℃ to 1100 ℃ at a speed of 30-50 ℃/min, and is cooled from 1100 ℃ to room temperature at a speed of 5-10 ℃/min, so as to obtain the high-entropy ceramic block material.
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