CN114349502B - Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof - Google Patents
Titanium-doped lanthanum hafnate ceramic for low-thermal-expansion thermal/environmental barrier coating and preparation method thereof Download PDFInfo
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Abstract
The invention provides titanium-doped lanthanum hafnate ceramic for a low-thermal-expansion thermal/environmental barrier coating and a preparation method thereof. The preparation method comprises the steps of firstly dissolving lanthanum oxide powder, hafnium oxide powder and titanium dioxide powder in absolute ethyl alcohol and carrying out ball milling to obtain mixed slurry, drying the mixed slurry to obtain mixed precursor powder, and carrying out reaction on the mixed precursor powder in a high-temperature air atmosphere to obtain La2(Hf1‑xTix)2O7Ceramic powder of which the molar fraction is 0<x is less than or equal to 0.2. The material for the coating has lower thermal expansion coefficient, is more matched with a ceramic matrix composite substrate, and has the advantages of simple preparation process, lower cost, higher product purity and wide application prospect.
Description
Technical Field
The invention relates to the technical field of ceramic matrix composite surface thermal/environmental barrier coating materials, in particular to titanium-doped lanthanum hafnate ceramic for a low-thermal-expansion thermal/environmental barrier coating.
Background
The aircraft engine is one of the most central parts of the modern aviation industry, and the demand for high-performance aircraft engines is continuously increasing in both military and civil fields, and the development of the engines towards high thrust and high thrust-weight ratio is a necessary trend, and the turbine inlet temperature of the engines is required to be continuously increased. The temperature resistance limit of the traditional high-temperature alloy material for manufacturing the hot end parts of the blades and the like is only 1100 ℃, and the requirements of a new generation of aeroengines cannot be met. Therefore, researchers have sought new refractory materials from ceramic matrix composites, the most prominent of which is SiCfthe/SiC composite material has the characteristics of excellent high-temperature stability, strong high-temperature oxidation resistance, low density, excellent high-temperature mechanical property, excellent chemical corrosion resistance and the like, and is one of the materials which have the most potential to replace nickel-based high-temperature alloy to prepare the hot-end component of the aero-engine.
SiCfAlthough the/SiC composite material has excellent oxidation resistance, it is susceptible to oxidation corrosion in the presence of high-temperature water vapor, generally referred to as water-oxygen corrosion, and turbine engine blades and the like contain a large amount of water vapor in the high-temperature gas environment in which they operate, and react to form volatile si (oh) under water-oxygen corrosionxCausing material loss and seriously affecting the service performance and service life. To solve this problem, a coating for resisting corrosive substances in such a working environment, namely an Environmental Barrier Coating (EBC), has been developed. By spraying or depositing on SiCfPreparing an environmental barrier coating on the surface of a component made of the/SiC composite material, and isolating the matrix from the external environment to form a barrier so as to protect the SiCfa/SiC composite material. Therefore, the material of the environmental barrier coating is generally selected from materials with better water and oxygen corrosion resistance. On the other hand, the development and application of environmental barrier coatings is readily linked to Thermal Barrier Coatings (TBCs), both to address the need for elevated service temperatures for aircraft engines, which have a relatively long history of development. The thermal barrier coating is used for solving the problem of insufficient temperature resistance of the high-temperature alloy, namely a coating with a heat insulation effect is prepared on the surface of an alloy matrix by using a material with low heat conductivity, so that the actual bearing temperature of the alloy matrix is reduced, and the upper temperature resistance limit of the whole component is improved. Thus, the primary function of the thermal barrier coating is thermal insulation, and the material selected is required to have a relatively low thermal conductivity. The application experience of the thermal barrier coating is provided, in order to further improve the SiCfThe service temperature of the/SiC composite material component and the concept of the thermal/environmental barrier coating are provided, namely, a thermal barrier coating is prepared on the basis of the environmental barrier coating, and the thermal/environmental barrier composite coating is formed, so that the thermal protection is provided while the environmental corrosion protection is provided. The NASA in the united states has developed and achieved some success for this composite coating, and it is anticipated that the thermal/environmental barrier coating will become a thermal/environmental barrier coatingThe key technology of the application of the ceramic-based high-performance aeroengine material in the future.
The thermal barrier layer in the thermal/environmental barrier coating system also serves as a thermal barrier, but is distinguished from conventional thermal barrier coatings primarily due to the difference in the substrate materials. The thermal expansion coefficients of the coating material and the base material are generally different, and the difference causes thermal mismatch stress in the thermal cycle process, so that the coating is cracked and fails in protection seriously. Therefore, in practical application, the thermal expansion matching between the coating material and the base material must be considered, and the difference is minimized as much as possible, which is the primary requirement that the coating can be stably used for a long time and exert a protective effect. The traditional thermal barrier coating protects an alloy matrix, and the alloy material has a high thermal expansion coefficient (12-15 multiplied by 10)-6K-1) The thermal expansion coefficient of the ceramic material of the thermal barrier coating is usually much lower than that of the alloy, so that it is desirable to choose the thermal expansion coefficient as high as possible for the material of the thermal barrier coating used for the alloy substrate; for acting on SiCfFor the coating on the/SiC composite, the SiC is usedfthe/SiC composite material has a low thermal expansion coefficient (4-5 multiplied by 10)-6K-1) This requires that both the environmental barrier layer and the thermal barrier layer material should also have a low coefficient of thermal expansion, which is an essential difference between thermal/environmental barrier coating materials and conventional thermal barrier coatings. Therefore, although the research method and technology of the traditional thermal barrier coating can be used for reference, the traditional thermal barrier coating material cannot be directly applied to SiCfOn the/SiC composite material, a thermal barrier layer material with a lower thermal expansion coefficient must be developed and designed.
The most typical conventional thermal barrier material is Yttria Stabilized Zirconia (YSZ), but it has low service temperature and high thermal expansion coefficient (10-12 × 10)-6K-1). In recent years, a number of new thermal barrier coating materials have gained widespread attention, the most promising of which is a having a pyrochlore or fluorite structure2B2O7The type compound, such as rare earth zirconate, rare earth hafnate, rare earth cerate, etc., has the characteristics of low thermal conductivity, lower thermal expansion coefficient than YSZ, excellent high-temperature stability, etc., and is applied toPotential materials for thermal/environmental barrier coatings. Another characteristic of the compound is that the ratio of the cationic radius of the A site to the cationic radius of the B site can cause the structure and performance of the material to change regularly when r (A)3+)/r(B4+) In the range of = 1.46 to 1.78, the material has a pyrochlore structure and r (A) is generally in this range3+)/r(B4+) The larger the value, the smaller the material thermal expansion coefficient, making it feasible to use doping modification to further reduce the thermal expansion coefficient.
Disclosure of Invention
Aiming at the performance requirements of a thermal barrier coating material applied to a thermal/environmental barrier coating, the invention provides a thermal/environmental barrier coating component, which is Ti element doped modified lanthanum hafnate powder with a molecular formula of La2(Hf1-xTix)2O7Wherein x has a value in the range of 0<x is less than or equal to 0.2, the preparation process is simple, the thermal expansion coefficient is low, and the aim is to utilize Ti with small radius4+Substituted La2Hf2O7Part of Hf4+A solid solution with a single pyrochlore phase is formed and the coefficient of thermal expansion is reduced, meeting the requirement of a thermal/environmental barrier coating for a low thermal expansion material.
The technical scheme of the invention is as follows: the invention firstly provides a low-thermal-expansion ceramic material for titanium-doped lanthanum hafnate thermal/environmental barrier coating, which has the molecular formula as follows: la2(Hf1-xTix)2O7It is prepared by using Ti element to La2Hf2O7Performing Hf4+Ion site substitution, wherein the value range of x is as follows: 0<x is less than or equal to 0.2; the La2Hf2O7Lanthanum hafnate, which has a cubic pyrochlore structure.
The invention also provides a preparation method of the ceramic material for the titanium-doped lanthanum hafnate thermal/environmental barrier coating with low thermal expansion, which comprises the following steps:
s1, mixing lanthanum oxide (La) according to a preset doping proportion2O3) Powder, hafnium oxide (HfO)2) Powder and titanium dioxide (TiO)2) Weighing and mixing the powder according to the converted mass ratio;
s2, dissolving the mixed powder in the step S1 in absolute ethyl alcohol, mixing and ball-milling to obtain uniformly mixed slurry;
s3, drying and sieving the slurry obtained in the step S2 to obtain pre-sintered powder;
s4, carrying out high-temperature reaction on the powder in the step S3 under a non-pressure condition, namely heating to 1450-1650 ℃ at a heating rate of 1-15 ℃/min, preserving heat for 6-16 h (the heat preservation temperature and the duration in the range can be in an inverse proportion relation), cooling to 500-800 ℃ at a rate of 1-15 ℃/min, and cooling to room temperature along with the furnace to obtain La2(Hf1-xTix)2O7Coarse powder;
s5, ball-milling the coarse powder obtained in the step S4, and sieving and separating to obtain fine ceramic powder with the particle size of less than 10 microns.
Further, in step S2, the ratio of the mixed powder to the absolute ethyl alcohol is: 1 g: (0.8-1.2 g), the ball milling time is 6-12 h, the ball milling tank adopted by ball milling is made of polyurethane, alumina or zirconia, the ball milling beads adopted by ball milling are made of polyurethane, alumina or zirconia, and the ball milling rotating speed is 300-400 rpm.
Further, in the step S3, the drying temperature is 80 to 120 ℃, and the mesh number of the screen is 200 to 500 meshes.
Further, in the step S4, the temperature rising rate is 5 ℃/min to 10 ℃/min, the temperature rises to 1500 ℃ to 1600 ℃, and the heat preservation time is 8 to 12 hours (the heat preservation temperature and the time length in this range may be in an inverse relationship).
Further, in the step S4, the cooling rate is 4 ℃/min to 10 ℃/min, and the temperature is reduced to 700 ℃ to 800 ℃ and then the furnace is cooled.
Compared with the prior art, the invention has the advantages that;
1. the invention provides titanium-doped lanthanum hafnate ceramic for a low-thermal-expansion thermal/environmental barrier coating, aiming at the protection problem of the existing ceramic matrix composite material in the field of aeroengines. The material replaces partial hafnium ions with titanium ions in a pyrochlore lattice of lanthanum hafnate with low thermal conductivity, and reduces the average radius of quadrivalent cations in the crystalMeanwhile, the original basic pyrochlore crystal lattice is not damaged, and a solid solution structure with a single crystal phase is formed. By utilizing the relationship between the ionic radius ratio of pyrochlore structural material and thermophysical property, the thermal expansion coefficient of the material is reduced, and the material can better react with SiC with low thermal expansion coefficientfThe matrix matching of the/SiC composite material can theoretically improve the temperature resistance of the ceramic matrix composite material, has better cycle life and can meet the service requirement.
The invention provides a preparation method of titanium doped lanthanum hafnate ceramic for a low-thermal-expansion thermal/environmental barrier coating. The method utilizes common oxide powder of lanthanum, hafnium and titanium elements, fully ball-milling and mixing the common oxide powder, reacting the mixture at a certain temperature for a certain time, and grinding and refining the mixture to obtain the La with a single pyrochlore structure2(Hf1-xTix)2O7A solid solution powder. The La2(Hf1-xTix)2O7The preparation method of the thermal/environmental barrier coating material has the advantages of simple process, low equipment requirement, short time consumption, suitability for mass production, higher product purity, low product thermal expansion coefficient and the like, and is suitable for high-temperature thermal protection of SiC composite materials.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings of which:
FIG. 1 is an XRD pattern of Ti doped lanthanum hafnate prepared in example 1 of the present invention;
fig. 2 is a microscopic examination chart of Ti-doped lanthanum hafnate prepared in example 1 of the present invention, wherein (a) is an SEM image of powder; (b) analyzing a Ti element distribution diagram for the energy spectrum of the powder, and reflecting the Ti element distribution in bright pixel points;
FIG. 3 is a thermal expansion rate curve diagram of Ti-doped lanthanum hafnate prepared in example 1 of the present invention at 30-1300 ℃.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following detailed description of the invention is provided in conjunction with the accompanying drawings and the detailed description of the invention.
Example 1
A low thermal expansion material for thermal/environmental barrier coating of titanium doped lanthanum hafnate and a preparation method thereof, comprising the following steps:
s1, according to La2(Hf1-xTix)2O7Taking the value of x as 0.1, and respectively weighing La2O3Powder, HfO2Powder and TiO2Powder, which is prepared into mixed powder with the total mass of 100 g;
s2, ball-milling the powder obtained in the step S1 with 100g of absolute ethyl alcohol, drying the slurry at the rotation speed of 300 r/min for 12 hours at the temperature of 110 ℃ to obtain pre-reaction powder;
s3, reacting the mixed powder obtained in the step S2 at a high temperature under a non-pressure air atmosphere, heating to 1500 ℃ at a speed of 5 ℃/min, and preserving heat for 12h to obtain La2(Hf1-xTix)2O7A solid solution powder;
s4, ball-milling the solid solution powder obtained in the step S3 (360 r/min, 24 h) to obtain fine powder;
la obtained by the above-mentioned production method2(Hf1-xTix)2O7The ceramic powder is measured by the following method:
(1) manually dry-pressing the powder in the step S4 for forming, wherein the pressure is 30 MPa, the pressure is maintained for 60-90S, the die is square, the side length is 30 mm, and the thickness of the pressed sheet is 5-6 mm;
(2) sintering the medium block pressing sheet in the step (1) in an air atmosphere, heating to 1600 ℃ at the speed of 3 ℃/min, preserving heat for 4h, cooling to 800 ℃ at the speed of 5 ℃/min, and then cooling along with the furnace;
(3) cutting the blocks in the step (2) into strip samples with the length of 25 mm +/-0.1 mm, wherein the surfaces are required to be flat and smooth;
(4) testing the linear thermal expansion rate of the strip sample in the step (3) at the temperature of 30-1300 ℃, wherein the heating rate is 10 ℃/min, and the formula is utilizedα=∆L/(L·∆T) The average linear thermal expansion coefficient was calculated.
The thermal/environmental barrier coating obtained in this example had a phase composition of a Ti-doped lanthanum hafnate material,The micro-topography and thermophysical properties are shown in figures 1 to 3, respectively. As can be seen from fig. 1, the product is substantially pure phase, and the superstructure peaks located in the (111), (311) and (511) crystal planes show that the material is a cubic pyrochlore structure. La prepared as shown in FIG. 2 (a)2(Hf1-xTix)2O7The microscopic morphology of a scanning electron microscope of a compact block obtained by sintering the solid solution powder can show that the material has clean grain boundary and no impurity phase; FIG. 2 (b) shows the distribution of Ti element obtained by EDS energy spectrum analysis, which shows that the doping element Ti of the prepared material is uniformly distributed on the whole level, and no local segregation or grain boundary enrichment phenomenon occurs, which proves that the introduced Ti atom is basically and completely dissolved into pyrochlore lattice, and that the prepared La is2(Hf1-xTix)2O7The material purity is high, and the raw material utilization rate is high. Fig. 3 shows that the thermal expansion rate of the material for the Ti-doped lanthanum hafnate thermal/environmental barrier coating obtained in the present embodiment is substantially linearly increased in the range of 30 to 1300 ℃, which indicates that the material has good high-temperature stability and no phase change occurs in the test temperature range; the calculated average coefficient of thermal expansion was 7.08X 10-6K-1Lower than most conventional thermal barrier coating ceramic materials, such as YSZ (11X 10)-6K-1) Or lanthanum zirconate (9.6X 10)-6K-1）。
Example 2
A low thermal expansion material for thermal/environmental barrier coating of titanium doped lanthanum hafnate and method of preparation, substantially the same as in example 1, except that: in the step S1, x is 0.2;
the detection proves that the La with a single pyrochlore structure is obtained in the embodiment2(Hf0.8Ti0.2)2O7Has high purity, and has an average thermal expansion coefficient of 6.65 x 10 at 30-1300 deg.C-6K-1。
Comparative example 1
A low thermal expansion material for thermal/environmental barrier coating of titanium doped lanthanum hafnate and its preparation method are the same as example 1 except that the doping fraction of Ti element x =0.
Undoped hafnate obtained in this comparative exampleLanthanum (La)2Hf2O7) Is of a cubic pyrochlore structure and has an average linear thermal expansion coefficient of 8.76 multiplied by 10 within the range of 30-1300 DEG C-6K-1It can be seen that the thermal expansion coefficient of the product of this comparative example is higher than that of example 1, which demonstrates that doping with a small radius of Ti element successfully lowers the thermal expansion coefficient of the material.
Comparative example 2
A material for a low thermal expansion titanium-doped lanthanum hafnate thermal/environmental barrier coating and a preparation method thereof, which are the same as the material in the embodiment 1 except that the doping fraction x =0.3 of the Ti element.
The phase composition of the Ti element doped lanthanum hafnate ceramic prepared by the comparative example is detected to be a small amount of La belonging to a perovskite structure besides a pyrochlore phase2Ti2O7It is shown that the purity of the product is lower than that of example 1, because when the doping fraction of Ti element is too high, the degree of lattice distortion is larger, the material can not maintain the original pyrochlore structure, and La is generated2Ti2O7To achieve a more stable state.
Comparative example 3
A low thermal expansion material for thermal/environmental barrier coating of titanium doped lanthanum hafnate and method of preparation, substantially the same as in example 1, except that: in step S3, the temperature is raised to 1400 ℃, and the heat preservation time is 8 h.
The phase composition of the Ti element doped lanthanum hafnate thermal/environmental barrier coating material prepared by the comparative example not only has a cubic pyrochlore phase, but also has obvious oxide inclusions such as La2O3、HfO2Etc., the product purity was lower than in example 1. This is because the holding temperature and time are both reduced, the reaction between the oxides does not proceed sufficiently, the atoms do not diffuse sufficiently, and the pyrochlore lattice cannot be completely dissolved.
Example 3
A low thermal expansion material for thermal/environmental barrier coating of titanium doped lanthanum hafnate and method of preparation, substantially the same as in example 1, except that:
in the step S3, the temperature is raised to 1600 ℃, and the heat preservation time is 8 h;
using an X-ray diffraction method, selecting a (622) diffraction peak as a reference, and calculating the thermal expansion coefficient of the microscopic layer by using diffraction peak shift, wherein the formula is as follows:
the detected substance is single pyrochlore structure La2(Hf0.9Ti0.1)2O7And the purity is higher. Table 1 shows La obtained in this example2(Hf1-xTix)2O7(x = 0.1) temperature-changing XRD data at room temperature to 1300 ℃ comprises 2 theta, crystal face spacing and lattice parameters, and it can be seen that as the temperature rises, the material expands due to heating, and the microscopic layer shows lattice expansion, namely, the crystal face spacing increases and the lattice parameters increase, and according to the Bragg equation 2dsin theta = lambda, the diffraction peak shifts towards a small angle. Calculating the average thermal expansion coefficient alpha of 7.26 multiplied by 10 at the room temperature to 1300 ℃ according to a formula-6K-1。
Table 1 temperature-variable XRD data for Ti-doped (x = 0.1) lanthanum hafnate materials
Comparative example 4
A low thermal expansion material for thermal/environmental barrier coating of titanium doped lanthanum hafnate and method of preparation, substantially the same as in example 3, except that:
the doping fraction x =0 of the Ti element in step S1;
undoped lanthanum hafnate (La) obtained in this comparative example2Hf2O7) The lattice parameters and the microscopic thermal expansion coefficients calculated by XRD are shown in Table 2 for a cubic pyrochlore structure, substantially pure phase.
Table 2 shows La obtained in this example2Hf2O7The variable-temperature XRD data at room temperature to 1300 ℃ comprises 2 theta, crystal face spacing and lattice parameters, and the change rule is the same as that of example 3, butThe smaller the initial diffraction angle, which indicates a smaller lattice constant for lanthanum hafnate doped with titanium, which is Ti, according to the Bragg equation4+Radius less than Hf4+The reason for that; in addition, it can be seen from the comparison with Table 1 that the parameters related to undoped lanthanum hafnate are more varied, which means that the thermal expansion is more remarkable, reflecting that La2Hf2O7La having a higher coefficient of thermal expansion than that of example 22(Hf0.9Ti0.1)2O7. Compared with the example 3, the average thermal expansion coefficient of the undoped lanthanum hafnate in the range of room temperature to 1300 ℃ is 8.82 multiplied by 10 according to the formula-6K-1Higher than La2(Hf0.9Ti0.1)2O7。
TABLE 2 temperature-variable XRD data for undoped lanthanum hafnate
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments to equivalent variations, without departing from the scope of the invention, using the teachings disclosed above. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (5)
1. A method of preparing a titanium doped lanthanum hafnate ceramic for low thermal expansion thermal/environmental barrier coatings comprising the steps of:
s1, the molecular formula composition of the titanium doped lanthanum hafnate ceramic is shown as follows: la2(Hf1-xTix)2O7It is prepared by using Ti element to La2Hf2O7Performing Hf4+Ion site substitution, wherein the value range of x is as follows: 0<x≤0.2According to a preset doping proportion, weighing and mixing lanthanum oxide powder, hafnium oxide powder and titanium dioxide powder according to the converted mass ratio;
s2, dissolving the mixed powder in the step S1 in absolute ethyl alcohol, mixing and ball-milling to obtain uniformly mixed slurry;
s3, drying and sieving the slurry obtained in the step S2 to obtain pre-sintered powder;
s4, carrying out high-temperature reaction on the powder in the step S3 under a non-pressure condition, wherein the high-temperature reaction is that the temperature is increased to 1450-1650 ℃ at the temperature increase rate of 1-15 ℃/min, the temperature is kept for 6-16 h, the temperature is reduced to 500-800 ℃ at the rate of 1-15 ℃/min, and finally the temperature is cooled to room temperature along with the furnace to obtain La2(Hf1-xTix)2O7Coarse powder;
s5, performing ball milling on the coarse powder obtained in the step S4, and sieving and separating to obtain fine ceramic powder with the particle size of less than 10 microns;
the La thus obtained2Hf2O7Lanthanum hafnate, which has a cubic pyrochlore structure.
2. The method of claim 1, wherein in step S2, the ratio of the mixed powder to the absolute ethyl alcohol is: 1 g: (0.8-1.2 g); the ball milling time is 6-12 h, and the ball milling tank adopted by ball milling is made of polyurethane, alumina or zirconia; the ball milling beads adopted by the ball milling are made of polyurethane, alumina or zirconia, and the ball milling rotating speed is 300-400 rpm.
3. The method for preparing titanium-doped lanthanum hafnate ceramic for a low thermal expansion thermal/environmental barrier coating according to claim 1, wherein the drying temperature is 80 to 120 ℃ and the mesh number of the screen is 200 to 500 in the step S3.
4. The method for preparing titanium-doped lanthanum hafnate ceramic for the low thermal expansion thermal/environmental barrier coating according to claim 1, wherein in the step S4, the temperature rise rate is 5 ℃/min to 10 ℃/min, the temperature rise rate is 1500 to 1600 ℃, and the holding time is 8 to 12 h.
5. The method for preparing titanium-doped lanthanum hafnate ceramic for the low thermal expansion thermal/environmental barrier coating according to claim 1, wherein in the step S4, the cooling rate is 4 ℃/min to 10 ℃/min, and the ceramic is cooled to 700 ℃ to 800 ℃ and then cooled with a furnace.
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