CN110606740A - High-entropy rare earth hafnate ceramic material and preparation method thereof - Google Patents
High-entropy rare earth hafnate ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of extreme environment thermal barrier and environmental barrier ceramic materials, in particular to a high-entropy rare earth hafnate (RE ') with low thermal conductivity'0.2RE"0.2Ho0.2Er0.2Tm0.2)4Hf3O12Ceramic materials and methods for their preparation. The chemical formula of the high-entropy rare earth hafnate is (RE'0.2RE"0.2Ho0.2Er0.2Tm0.2)4Hf3O12Wherein RE 'is La or Yb, and RE' is Gd or Lu. The preparation process specifically comprises the following steps: lanthanum oxide powder, gadolinium oxide powder, holmium oxide powder, erbium oxide powder, thulium oxide powder, ytterbium oxide powder, lutetium oxide powder and hafnium oxide powder are used as raw materials, mixed by a wet method and sintered under no pressure in an air atmosphere; and sintering in a hot pressing furnace with protective atmosphere to obtain the high-entropy rare earth hafnate material. The invention prepares (RE ') with high purity and low thermal conductivity'0.2RE"0.2Ho0.2Er0.2Tm0.2)4Hf3O12A ceramic material.
Description
Technical Field
The invention relates to the field of extreme environment thermal barrier and environmental barrier ceramic materials, in particular to a high-entropy rare earth hafnate (RE ') with low thermal conductivity'0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12Ceramic material and preparation method thereofThe method is carried out.
Background
The high thrust-weight ratio aircraft engine thermal structure component faces extreme gas environment, the development of the multifunctional thermal barrier/environmental barrier integrated coating with excellent comprehensive performance can meet the composite requirement of the thermal barrier coating and the environmental barrier coating of the ceramic matrix composite thermal structure component in the extreme gas environment of the aircraft, and the thrust-weight ratio and the long-term service stability of the engine are greatly improved. Yttria Stabilized Zirconia (YSZ) and rare earth zirconates (RE)2Zr2O7) Due to its good thermal insulation properties, it is a thermal barrier coating that is widely used at present. Compared with rare earth zirconate, the rare earth hafnate has higher melting point and can be used at higher temperature; hafnates of the same rare earth elements exhibit lower coefficients of thermal expansion than zirconates, matching ceramic matrix composites; and fluorite structured rare earth hafnate (RE)4Hf3O12) The content of the medium rare earth elements is higher, and the medium rare earth elements are expected to have more excellent environmental corrosion resistance; so that the rare earth hafnate has more advantages when being applied as a protective coating of a ceramic component (W.P.Hu, et al.J. Mater.Sci.Technol (journal of materials science and technology): 2019(35) 2064-.
In recent years, a new class of materials known as Entropy stabilized oxides (entropically stabilized oxides) has attracted considerable attention by researchers, defined as single phase complex solid solutions (y.f. ye, et al. mater. today's materials) containing multiple major elements (five or more) in "equimolar or near equimolar ratios" (y.f. ye, et al. mater. today's materials) 2016(19) 349-362). There are reports in the literature that various fluorite-structured single-phase solid solutions with high configuration entropy are prepared by spark plasma sintering, and these high-entropy fluorite oxides exhibit high hardness, low electrical conductivity, and excellent low thermal conductivity (j.gild, et al.j.euro.series.soc. (published european ceramics society of china) 2018(38) 3578-. The entropy-stabilized oxide can enrich the diversity of materials and exhibit excellent properties. The invention synthesizes the high-entropy rare earth hafnate with a defect fluorite structure: (RE'0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12Based on Ho, Er and Tm capable of forming a defective fluorite structureLa and Gd with larger radius or Yb and Lu with smaller radius are respectively introduced, and the material performance is improved through the atomic size and mass difference effect.
Disclosure of Invention
The purpose of the invention is to provide high-entropy rare earth hafnate (RE'0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12Ceramic materials and methods for their preparation.
The technical scheme of the invention is as follows:
a high-entropy rare earth hafnate ceramic material has a chemical formula of (RE'0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12Wherein RE 'is La or Yb, and RE' is Gd or Lu.
The preparation method of the high-entropy rare earth hafnate ceramic material comprises the following specific steps:
1) lanthanum oxide powder, gadolinium oxide powder, holmium oxide powder, erbium oxide powder, thulium oxide powder, ytterbium oxide powder, lutetium oxide powder and hafnium oxide powder are taken as raw materials;
(RE′0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12middle (RE'0.2RE″0.2Ho0.2Er0.2Tm0.2): hf: the molar ratio of O is 4: 3: 12, wherein RE': RE': ho: er: molar ratio of Tm 0.2: 0.2: 0.2: 0.2: 0.2;
2) taking ethanol as a medium, carrying out ball milling and mixing on the original powder for 5-24 hours to form slurry, drying and sieving the slurry to obtain powder, and synthesizing the powder in a muffle furnace at no pressure, wherein the heating rate is 5-15 ℃/min, the synthesis temperature is 1500-1650 ℃, the synthesis time is 0.5-1.5 hours, and finally obtaining the high-entropy rare earth hafnate ceramic powder;
3) the pressureless synthesized high-entropy rare earth hafnate ceramic powder is subjected to ball milling for 10-24 hours by a physical mechanical method, is placed into a graphite mold for cold press molding, and is subjected to hot press sintering in a hot press furnace with a protective atmosphere, wherein the heating rate is 5-20 ℃/min, the sintering temperature is 1600-1750 ℃, the sintering time is 0.5-2 hours, and the sintering pressure is 20-40 MPa.
According to the preparation method of the high-entropy rare earth hafnate ceramic material, the original particle size ranges of lanthanum oxide powder, gadolinium oxide powder, holmium oxide powder, erbium oxide powder, thulium oxide powder, ytterbium oxide powder, lutetium oxide powder and hafnium oxide powder are 100-800 meshes.
The preparation method of the high-entropy rare earth hafnate ceramic material adopts the pressureless synthesis under the air atmosphere at normal pressure.
According to the preparation method of the high-entropy rare earth hafnate ceramic material, the protective atmosphere adopted by hot-pressing sintering is argon or helium.
The preparation method of the high-entropy rare earth hafnate ceramic material adopts wet ball milling in an alcohol medium by a physical mechanical method.
The design idea of the invention is as follows: from the perspective of material structure design, multiple rare earth elements are introduced into the rare earth hafnate, and the Gibbs free energy of the system can be effectively reduced by utilizing the high entropy effect, namely the high mixed entropy under the high temperature condition, so that a stably generated single phase is obtained; from the design angle of material performance, the properties of the material are compounded by selecting various specific rare earth elements; the different sizes of various rare earth atoms are utilized to cause serious lattice distortion, thereby bringing about physical, chemical and mechanical properties superior to those of the traditional solid solution.
The invention has the advantages and beneficial effects that:
1. high purity and high-temp stability. For the high-entropy material, the purity and the phase stability are the key points of the application, and the high-entropy rare earth hafnate prepared by the method is prepared by in-situ solid solution of a plurality of rare earths to fluorite structure rare earth hafnate (RE)4Hf3O12) Contains no impurity phase. The sintering temperature reaches 1750 ℃, the high-entropy rare earth hafnate still keeps good structural stability, and the application requirements of thermal barrier and barrier-surrounding coatings in the field of aviation can be met.
2. The thermal property is excellent. In the present invention, the high entropy rare earth hafnate has enhanced interatomic bonding and a thermal expansion coefficient compared with single rare earth hafnate (e.g. Ho)4Hf3O12Etc.) is remarkably reduced, which is beneficial to improving the thermal stress matching of the environmental barrier coating and the ceramic substrate and prolonging the service life of the coating. In addition, the high-entropy rare earth hafnate contains various rare earth atoms, the mass and size difference is large, the phonon mean free path is reduced, the thermal conductivity of the material can be obviously reduced, and the functional integration of a thermal barrier/environmental barrier coating is hopeful to realize.
Drawings
FIG. 1 shows the crystal morphology and element distribution of high-entropy rare earth hafnate after hot corrosion. Wherein (a) is the crystal grain shape graph and element (La, Gd, Ho, Er, Tm, Hf) distribution of F-1, and (b) is the crystal grain shape graph and element (Yb, Lu, Ho, Er, Tm, Hf) distribution of F-2.
FIG. 2 (RE'0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12X-ray diffraction pattern of (a). In the figure, the abscissa 2 θ represents the diffraction angle (Degree), and the ordinate Intensity represents the relative Intensity (arb.
FIG. 3 (RE'0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12The coefficient of thermal expansion of (a) is plotted against temperature. In the figure, the abscissa Temperature represents the Temperature (K) and the ordinate CTE represents the coefficient of thermal expansion (10)-6K-1)。
FIG. 4 (RE'0.2RE″0.2Ho0.2Er0.2Tm0.2)4Hf3O12Thermal conductivity versus temperature curve of (a). In the figure, the abscissa Temperature represents Temperature (K), and the ordinate Thermal conductivity represents Thermal conductivity (W m)-1K-1)。
Detailed Description
The present invention will be described in more detail below with reference to examples.
Example 1
In this example, the primary particle size of the raw materials, lanthanum oxide, gadolinium oxide, holmium oxide, erbium oxide, thulium oxide and hafnium oxide powder, was 600 mesh, and lanthanum oxide (4.8 g), gadolinium oxide (5.3 g), holmium oxide (5.54 g), erbium oxide (5.60 g), thulium oxide (5.65 g) and hafnium oxide (23.1 g) (in accordance with the chemical formula)Chemical formula (La)0.2Gd0.2Ho0.2Er0.2Tm0.2)4Hf3O12(defined as F x-1)), the powder was put into a silicon nitride ball mill pot for ball milling for 6 hours using absolute ethanol as a medium, and the dried powder was pressureless sintered in a muffle furnace. The sintering process comprises the following steps: heating to 1600 ℃ at the speed of 5 ℃/min, and preserving the heat for 2.5 hours to obtain the high-entropy rare earth hafnate ceramic powder. Putting the pressureless sintered high-entropy rare earth hafnate powder into a ball milling tank, carrying out ball milling for 10 hours by adopting a wet method under an alcohol medium, then drying, putting the dried powder into a graphite mold for cold press molding at room temperature, and finally putting the cold-pressed mold into a graphite sintering furnace for hot press sintering. The sintering atmosphere is argon, the temperature is increased to 1700 ℃ at the speed of 5 ℃/min, the temperature is kept for 0.5 hour under the pressure of 20MPa, and then the furnace is cooled. The pressure in the whole heat preservation process is maintained at 20MPa, and the whole hot-pressing sintering process is carried out under the protection of argon.
As shown in FIG. 1(a), as can be seen from the crystal morphology and element distribution of the high-entropy rare earth hafnate after hot corrosion, the average size of F-LG crystal grains is about 0.5 μm, and by performing surface scanning analysis on the sample surface, the La, Gd, Ho, Er, Tm and Hf elements are uniformly distributed, and no segregation of the elements, that is, the formation of a second phase, is caused. As shown in FIG. 2, the obtained reaction product was pure (La) by X-ray diffraction analysis0.2Gd0.2Ho0.2Er0.2Tm0.2)4Hf3O12。
Example 2
In this example, the original particle size of the raw materials of holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and hafnium oxide powder was 200 mesh, and 5.37 g of holmium oxide, 5.44 g of erbium oxide, 5.49 g of thulium oxide, 5.60 g of ytterbium oxide, 5.66 g of lutetium oxide and 22.44 g of hafnium oxide (corresponding to the chemical formula (Ho) were added0.2Er0.2Tm0.2Yb0.2Lu0.2)4Hf3O12(defined as F x-2)), using absolute ethyl alcohol as a medium, placing the powder into a silicon nitride ball milling tank for ball milling for 24 hours, and sintering the dried powder in a muffle furnace without pressure. Sintering toolThe process comprises the following steps: heating to 1600 ℃ at the speed of 15 ℃/min, and preserving the heat for 1.5 hours to obtain the high-entropy rare earth hafnate ceramic powder. And putting the pressureless sintered powder into a ball milling tank, carrying out ball milling for 24 hours by adopting a wet method under an alcohol medium, then drying, putting the dried solid solution powder into a graphite mould for cold press molding at room temperature, and finally putting the cold pressed mould into a graphite sintering furnace for hot press sintering. The sintering atmosphere is argon, the temperature is increased to 1750 ℃ at the speed of 20 ℃/min, the temperature is kept for 2 hours under the pressure of 40MPa, and then the furnace is cooled. The pressure in the whole heat preservation process is maintained at 40MPa, and the whole hot-pressing sintering process is carried out under the protection of helium.
As shown in FIG. 1(b), it can be seen from the crystal morphology and element distribution of the high-entropy rare earth hafnate after hot corrosion that the average size of the crystal grains is about 1.1 μm, and by surface scanning analysis of the sample surface energy spectrum, it can be known that the Yb, Lu, Ho, Er, Tm and Hf elements are uniformly distributed, and no segregation of the elements, that is, the formation of the second phase, occurs. As shown in FIG. 2, the obtained reaction product was analyzed by X-ray diffraction to be pure (Ho)0.2Er0.2Tm0.2Yb0.2Lu0.2)4Hf3O12。
Comparative example
27.2 g of holmium oxide and 22.8 g of hafnium oxide (chemical formula: Ho)4Hf3O12) Single phase pure Ho was obtained according to the procedure used in example 14Hf3O12A ceramic.
As shown in FIG. 3, the coefficients of thermal expansion of three of the materials were first measured over a temperature range of 473K to 1673K, with the high entropy rare earth hafnate having a coefficient of thermal expansion that is relatively pure phase Ho4Hf3O12The method has the advantages that the method obviously reduces the cost, and the high-entropy rare earth hafnate material is used as a protective coating, thereby being beneficial to improving the thermal stress matching between the coating and the ceramic substrate and prolonging the service life of the coating.
As shown in FIG. 4, the thermal conductivity curves of the three materials with temperature were further measured by the excited scintillation method, and Ho in the measured temperature range4Hf3O12The thermal conductivity of the ceramic is 1.6 W.m-1·K-1Is a typical low-conductivity materialHigh entropy rare earth hafnate (La)0.2Gd0.2Ho0.2Er0.2Tm0.2)4Hf3O12(defined as F x-1) thermal conductivity of about 1.4 W.m over the entire temperature range-1·K-1All are lower than single-component Ho4Hf3O12The ceramic, the high-entropy rare earth hafnate ceramic material has wide application prospect as a novel thermal barrier coating material.
The embodiment result shows that the pressureless/hot pressing two-step sintering method is adopted to prepare the high-entropy rare earth hafnate material with high purity and good high-temperature mechanical property, and the performance index range is as follows: purity of>99 wt%, coefficient of thermal expansion (8.58-9.05) x 10-6K-1(room temperature to 1473K) and a thermal conductivity of 1.41 to 1.82 W.m-1·K-1。
Claims (6)
1. A high entropy rare earth hafnate ceramic material is characterized in that the high entropy rare earth hafnate is of the chemical formula (RE'0.2RE"0.2Ho0.2Er0.2Tm0.2)4Hf3O12Wherein RE 'is La or Yb, and RE' is Gd or Lu.
2. A method for preparing a high entropy rare earth hafnate ceramic material of claim 1, comprising the steps of:
1) lanthanum oxide powder, gadolinium oxide powder, holmium oxide powder, erbium oxide powder, thulium oxide powder, ytterbium oxide powder, lutetium oxide powder and hafnium oxide powder are taken as raw materials;
(RE'0.2RE"0.2Ho0.2Er0.2Tm0.2)4Hf3O12middle (RE'0.2RE"0.2Ho0.2Er0.2Tm0.2): hf: the molar ratio of O is 4: 3: 12, wherein RE': RE': ho: er: molar ratio of Tm 0.2: 0.2: 0.2: 0.2: 0.2;
2) taking ethanol as a medium, carrying out ball milling and mixing on the original powder for 5-24 hours to form slurry, drying and sieving the slurry to obtain powder, and synthesizing the powder in a muffle furnace at no pressure, wherein the heating rate is 5-15 ℃/min, the synthesis temperature is 1500-1650 ℃, the synthesis time is 0.5-1.5 hours, and finally obtaining the high-entropy rare earth hafnate ceramic powder;
3) the pressureless synthesized high-entropy rare earth hafnate ceramic powder is subjected to ball milling for 10-24 hours by a physical mechanical method, is placed into a graphite mold for cold press molding, and is subjected to hot press sintering in a hot press furnace with a protective atmosphere, wherein the heating rate is 5-20 ℃/min, the sintering temperature is 1600-1750 ℃, the sintering time is 0.5-2 hours, and the sintering pressure is 20-40 MPa.
3. The preparation method of the high-entropy rare earth hafnate ceramic material as claimed in claim 2, wherein the primary particle size ranges of the lanthanum oxide powder, gadolinium oxide powder, holmium oxide powder, erbium oxide powder, thulium oxide powder, ytterbium oxide powder, lutetium oxide powder and hafnium oxide powder are 100-800 mesh.
4. A method of preparing a high entropy rare earth hafnate ceramic material of claim 2, wherein the pressureless synthesis is carried out at atmospheric pressure in an air atmosphere.
5. The method for preparing a high entropy rare earth hafnate ceramic material as claimed in claim 2, wherein the atmosphere for the hot press sintering is argon or helium.
6. The method for preparing a high entropy rare earth hafnate ceramic material as claimed in claim 2, wherein the ball milling is performed by physical mechanical method and wet ball milling is performed in alcohol medium.
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| CN111423236A (en) * | 2020-03-22 | 2020-07-17 | 华南理工大学 | (Hf) 0.25Ti0.25Zr0.25W0.25) N high-entropy ceramic powder and preparation method thereof |
| CN111892400A (en) * | 2020-08-18 | 2020-11-06 | 新沂市锡沂高新材料产业技术研究院有限公司 | High-transmittance high-entropy transparent ceramic and preparation method thereof |
| CN112778010A (en) * | 2020-12-31 | 2021-05-11 | 东华大学 | High-entropy ceramic with high hardness and high conductivity and preparation method and application thereof |
| CN113089135A (en) * | 2021-04-08 | 2021-07-09 | 齐鲁工业大学 | High-entropy zirconate inorganic fiber and preparation method thereof |
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| CN111423236A (en) * | 2020-03-22 | 2020-07-17 | 华南理工大学 | (Hf) 0.25Ti0.25Zr0.25W0.25) N high-entropy ceramic powder and preparation method thereof |
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| CN112778010A (en) * | 2020-12-31 | 2021-05-11 | 东华大学 | High-entropy ceramic with high hardness and high conductivity and preparation method and application thereof |
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Application publication date: 20191224 |