CN113024232B - Light-heavy rare earth mixed high-entropy rare earth silicate compact block and preparation method thereof - Google Patents
Light-heavy rare earth mixed high-entropy rare earth silicate compact block and preparation method thereof Download PDFInfo
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Abstract
The invention provides a light and heavy rare earth mixed high-entropy rare earth silicate compact block, which has the chemical formula as follows: (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5The block is represented by Ho2O3、Lu2O3、Yb2O3、Eu2O3、SiO2The material is prepared by wet mixing, high-temperature reaction, wet ball milling, cold press molding, cold isostatic pressing and high-temperature sintering. The light and heavy rare earth mixed high-entropy rare earth silicate compact block disclosed by the invention is high in solid solubility, good in high-temperature stability, high in density, simple in preparation method process, high in production efficiency, high in safety and energy-saving.
Description
Technical Field
The invention belongs to the technical field of ceramic materials for an aero-engine environmental barrier coating, and particularly relates to a light-heavy rare earth mixed high-entropy rare earth silicate compact block and a preparation method thereof.
Background
The thrust-weight ratio of the aircraft engine is a development direction of the future aircraft industry, and the temperature of a front inlet of a turbine is required to be increased to realize a high thrust-weight ratio, so that the working temperature of a combustion chamber, a turbine blade and other hot end parts is continuously increased. At present, the blade material of the aeroengine is a high-temperature alloy material, and the further temperature rise of the front inlet of the turbine reaches the temperature bearing limit of the nickel-based high-temperature alloy, so that the nickel-based high-temperature alloy is difficult to meet the working requirement of the engine. Silicon-based non-oxide ceramics and composite materials thereof (such as silicon-based ceramic materials) have excellent high-temperature thermal and mechanical properties, and are expected to replace traditional high-temperature alloys to be used as a new generation of hot end part materials of aircraft engines.
Under the dry combustion environment, a layer of SiO is generated on the surface of the silicon-based ceramic material2A film with good protection effect for preventing further oxygen from being introduced into the silicon-based materialAnd (4) transforming. However, in a combustion environment containing water vapor, the silicon-based ceramic reacts with the water vapor to form volatile Si (OH)4Causing degradation of material properties. The Environmental Barrier Coatings (EBC) have the characteristics of good molten salt corrosion resistance, water oxygen corrosion resistance and the like, and the problem can be hopefully solved by coating the EBC on the surface of a hot end part of an engine.
The rare earth silicate ceramic material has excellent steam corrosion resistance and CMAS (CaO-MgO-Al) resistance2O3-SiO2) Corrosion performance and low thermal expansion coefficient, and is a hot candidate material of a new generation of environmental barrier coating. Some rare earth monosilicates and rare earth disilicates meet the basic requirements as environmental barrier coatings for silicon-based non-oxide ceramics. However, the properties of single-phase rare earth silicates are not balanced in all aspects, and candidate materials which completely meet the performance requirements of environmental barrier coatings cannot be found at present, so that the materials need to be optimally designed.
The high-entropy ceramic is formed by applying the design idea of high-entropy alloy to ceramic and replacing single cations in the traditional ceramic with several equimolar or nearly equimolar cations. The self characteristics of various elements and the interaction among the elements can combine the excellent performances of the elements, so that the high-entropy ceramic has the excellent performances of all components. Common high-entropy ceramics are mainly high-entropy rare earth silicate blocks, such as high-entropy rare earth monosilicate (Yb) of heavy rare earth elements0.25Y0.25Lu0.25Er0.25)2SiO5Bulk, rare earth disilicate (Yb)0.2Y0.2Lu0.2Sc0.2Gd0.2)2Si2O7Bulk, rare earth monosilicate (Y)0.25Ho0.25Er0.25Yb0.25)2SiO5Blocks, and the like. However, the existing preparation method of the high-entropy rare earth silicate block has the problems of complex process, low efficiency, low density of the block, single type of rare earth elements (all heavy rare earth), and the like.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a light-heavy rare earth mixed high-entropy rare earth silicate compact block which is high in solid solubility, good in high-temperature stability and high in density, and the preparation method is simple in process, high in production efficiency, high in safety and energy-saving.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a light and heavy rare earth mixed high-entropy rare earth silicate compact block, which has the chemical formula as follows: (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5Wherein Ho (holmium), Lu (lutetium) and Yb (ytterbium) are heavy rare earth elements, and Eu (europium) is light rare earth element.
The invention also provides a preparation method of the light and heavy rare earth mixed high-entropy rare earth silicate compact block, which comprises the following steps:
s1, according to Ho2O3:Lu2O3:Yb2O3:Eu2O3:SiO2Weighing the raw materials according to the molar ratio of 1:1:1:1: 4;
s2, uniformly mixing the raw materials in the step S1 by adopting a wet mixing method, drying and sieving to obtain mixed raw materials;
s3, reacting the mixed raw materials obtained in the step S2 at high temperature to obtain light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles;
s4, carrying out wet ball milling on the heavy rare earth mixed high-entropy rare earth silicate ceramic particles obtained in the step S3, drying and sieving to obtain light rare earth mixed high-entropy rare earth silicate ceramic powder;
s5, carrying out cold press molding and cold isostatic pressing on the light and heavy rare earth mixed high-entropy rare earth silicate ceramic powder obtained in the step S4 to obtain a light and heavy rare earth mixed high-entropy rare earth silicate block blank;
and S6, sintering the light and heavy rare earth mixed high-entropy rare earth silicate block blank obtained in the step S5 at a high temperature to obtain a heavy rare earth mixed high-entropy rare earth silicate compact block.
Preferably, the wet mixing in step S2 takes ethanol as a medium, the rotation speed is 100-300r/min, and the time is 4-12 h.
Preferably, the high-temperature reaction in the step S3 is a reaction at 1500-1700 ℃ for 2-8h in an air atmosphere.
Preferably, the wet ball milling in step S4 uses ethanol as a medium, the rotation speed is 100-.
Preferably, the pressure of the cold press molding in the step S5 is 10-30MPa, and the dwell time is 1-5 min; the pressure of the cold isostatic pressing is 100-250MPa, and the pressure maintaining time is 10-30 min.
Preferably, the temperature of the high-temperature sintering in the step S5 is 1400-1750 ℃, and the holding time is 2-12 h.
Preferably, the Ho of step S12O3、Lu2O3、Yb2O3、Eu2O3、SiO2The purity of (A) is 99.9% -99.99%.
Preferably, the sieving in steps S2 and S4 is through a 40-120 mesh sieve.
Preferably, the ball milling pot and the ball milling ball of the wet mixing in step S2 and the wet ball milling in step S4 are both made of zirconia or agate.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a light and heavy rare earth mixed high-entropy rare earth silicate compact block, which has the chemical formula as follows: (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5The block is represented by Ho2O3、Lu2O3、Yb2O3、Eu2O3、SiO2The material is prepared by wet mixing, high-temperature reaction, wet ball milling, cold press molding, cold isostatic pressing and high-temperature sintering. The invention has the following advantages:
(1) the preparation process is simple in process, high in safety and energy-saving.
(2) In the preparation process of the light and heavy rare earth mixed high-entropy rare earth silicate compact block, the method of cold isostatic pressing and pressureless sintering is adopted, the production efficiency is high, and a plurality of samples can be prepared simultaneously: the common hot-pressing sintering can prepare only one sample at a time; the cold isostatic pressing and pressureless sintering method of the invention can be used for firing a plurality of samples in one furnace.
(3) The light and heavy rare earth mixed high-entropy rare earth silicate compact block disclosed by the invention is high in solid solubility, good in high-temperature stability and high in density, and can reach more than 96%.
Drawings
FIG. 1 shows (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5X-ray diffraction patterns of (a);
FIG. 2 is (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5Scanning electron microscope images of the surface;
FIG. 3 shows (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5Scanning electron microscope images of the fractures.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the respective embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The experimental procedures in the following examples were carried out by conventional methods unless otherwise specified, and the test materials used in the following examples were commercially available by conventional methods unless otherwise specified.
Example 1 dense block of light and heavy rare earth mixed high-entropy rare earth silicate
The chemical formula of the light-heavy rare earth mixed high-entropy rare earth silicate compact block is as follows: (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5Wherein Ho (holmium), Lu (lutetium) and Yb (ytterbium) are heavy rare earth elements, and Eu (europium) is light rare earth element.
The preparation method of the light and heavy rare earth mixed high-entropy rare earth silicate compact block comprises the following steps:
(1) according to Ho2O3:Lu2O3:Yb2O3:Eu2O3:SiO2Weighing raw materials according to the molar ratio of 1:1:1:1:4, Ho2O3、Lu2O3、Yb2O3、Eu2O3、SiO2The purity of the raw material is 99.9-99.99%;
(2) wet mixing the raw materials by using a ball mill, taking absolute ethyl alcohol as a medium, taking a ball milling tank and a grinding ball as zirconia or agate materials, mixing, drying and sieving by using a 80-mesh sieve to obtain a mixed raw material, wherein the rotating speed is 200r/min and the time is 8 h;
(3) placing the mixed raw materials in a high-temperature reaction furnace, and reacting for 5h at 1600 ℃ in the air atmosphere to obtain light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles;
(4) carrying out wet ball milling on the light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles, wherein the ball milling takes absolute ethyl alcohol as a medium, a ball milling tank and a milling ball are made of zirconia or agate materials, the rotating speed is 200r/min, the time is 8h, and the light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles are obtained by drying and sieving through a 80-mesh sieve after ball milling;
(5) cold press molding is carried out on the light rare earth and heavy rare earth mixed high-entropy rare earth silicate ceramic powder, the pressure of the cold press molding is 20MPa, and the pressure maintaining time is 3 min; then carrying out cold isostatic pressing, wherein the pressure of the cold isostatic pressing is 150MPa, and the pressure maintaining time is 20min, so as to obtain a light-heavy rare earth mixed high-entropy rare earth silicate block blank;
(6) placing the light and heavy rare earth mixed high-entropy rare earth silicate ceramic blocky blank into a high-temperature reaction furnace, sintering at 1650 ℃ for 8h in the air atmosphere to obtain a heavy rare earth mixed high-entropy rare earth silicate compact blocky body (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5。
For (Ho) prepared as described above0.25Lu0.25Yb0.25Eu0.25)2SiO5Performing X-ray diffraction spectrum analysis (with the mixed powder as a contrast),incident light is K alpha 1 ray of Cu filtered by a monochromator and has a wavelength of
The working voltage is 40kV, the working current is 45mA, and the scanning speed is 10 degrees/min. Wherein PDF #40-0383 is single-phase rare earth silicate Ho2SiO5The mixed powder is Ho2SiO5、Lu2SiO5、Yb2SiO5、Eu2SiO5Mechanically mixing four kinds of rare earth silicate according to an equal molar ratio.
As can be found from the diffraction pattern of FIG. 1, (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5The peak of (A) is consistent with that of a standard PDF card, and the peak position is shifted only due to the lattice distortion of the high-entropy ceramic; the peaks of the mixed powder almost match those of the PDF card, but if the mixed powder is observed in a certain angle range under magnification, the mixed powder is found to have distinct peaks, for example, 21 ° to 24 ° and 27 ° to 29 °, indicating that there are a plurality of phases in the mixed powder. Prepared in this example (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5The pure-phase light-heavy rare earth mixed high-entropy rare earth silicate is free of impurities and high in solid solubility, and is not a mechanical mixture of several kinds of rare earth silicates. In addition, although the preparation temperature of the sample is high and the preparation time is long, other reactions do not occur to generate impurities, which indicates that the high-temperature stability of the sample is good.
At the same time, scanning electron microscope (SU8010) was used to prepare (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5The surface of (2) was scanned by electron microscopy, and as can be seen from the results in FIG. 2, the sample surface was very dense with few voids.
Scanning electron microscope (SU8010) is used to measure the (Ho) obtained0.25Lu0.25Yb0.25Eu0.25)2SiO5The fracture of the sample is subjected to electron microscope scanning, and as can be seen from the result of fig. 3, the fracture holes of the sample are very few, andthe pore diameters are all below 10 mu m, which shows that the density of the sample is very high.
In addition, for the prepared (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5And (3) carrying out density calculation: established using Materials Studio (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5Obtaining a cell of theoretical density rho0＝6.69934g/cm3(ii) a (Ho) of the present example was measured using Archimedes drainage method0.25Lu0.25Yb0.25Eu0.25)2SiO5Has a density of rho of 6.527g/cm3Density eta is rho/rho0
It can be calculated that (Ho) prepared in this example0.25Lu0.25Yb0.25Eu0.25)2SiO5The density (ratio of actual measured density to theoretical density) of 97.43%.
Example 2A dense block of light and heavy rare earth mixed high-entropy rare earth silicate
The chemical formula of the light and heavy rare earth mixed high-entropy rare earth silicate compact block is as follows: (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5Wherein Ho (holmium), Lu (lutetium) and Yb (ytterbium) are heavy rare earth elements, and Eu (europium) is light rare earth element.
The preparation method of the light and heavy rare earth mixed high-entropy rare earth silicate compact block comprises the following steps:
(1) according to Ho2O3:Lu2O3:Yb2O3:Eu2O3:SiO2Weighing raw materials according to the molar ratio of 1:1:1:1:4, Ho2O3、Lu2O3、Yb2O3、Eu2O3、SiO2The purity of the raw material is 99.9-99.99%;
(2) wet mixing the raw materials by using a ball mill, taking absolute ethyl alcohol as a medium, taking a ball milling tank and a grinding ball as zirconia or agate materials, mixing, drying and sieving by using a 40-mesh sieve to obtain a mixed raw material, wherein the rotating speed is 100r/min and the time is 4 hours;
(3) placing the mixed raw materials in a high-temperature reaction furnace, and reacting at 1500 ℃ for 8h in the air atmosphere to obtain light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles;
(4) carrying out wet ball milling on the light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles, wherein the ball milling takes absolute ethyl alcohol as a medium, a ball milling tank and a milling ball are made of zirconia or agate materials, the rotating speed is 100r/min, the time is 12 hours, and the light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles are obtained by drying and sieving through a 40-mesh sieve after ball milling;
(5) cold press molding is carried out on the light rare earth and heavy rare earth mixed high-entropy rare earth silicate ceramic powder, the pressure of the cold press molding is 10MPa, and the pressure maintaining time is 5 min; then carrying out cold isostatic pressing, wherein the pressure of the cold isostatic pressing is 100MPa, and the pressure maintaining time is 30min, so as to obtain a light-heavy rare earth mixed high-entropy rare earth silicate block blank;
(6) placing the light and heavy rare earth mixed high-entropy rare earth silicate ceramic blocky blank into a high-temperature reaction furnace, sintering in the air atmosphere at 1400 ℃, and keeping the temperature for 12 hours to obtain a heavy rare earth mixed high-entropy rare earth silicate compact block (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5。
Prepared by this example (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5The X-ray diffraction result, the surface and fracture scanning electron microscope result of the composite material are consistent with those of the embodiment 1, and the compactness is more than 96%.
Example 3A dense block of light and heavy rare earth mixed high-entropy rare earth silicate
The chemical formula of the light and heavy rare earth mixed high-entropy rare earth silicate compact block is as follows: (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5Wherein Ho (holmium), Lu (lutetium) and Yb (ytterbium) are heavy rare earth elements, and Eu (europium) is light rare earth element.
The preparation method of the light-heavy rare earth mixed high-entropy rare earth silicate compact block comprises the following steps:
(1) according to Ho2O3:Lu2O3:Yb2O3:Eu2O3:SiO2Weighing raw materials according to the molar ratio of 1:1:1:1:4, Ho2O3、Lu2O3、Yb2O3、Eu2O3、SiO2The purity of the raw material is 99.9-99.99%;
(2) wet mixing the raw materials by using a ball mill, taking absolute ethyl alcohol as a medium, taking a ball milling tank and a grinding ball as zirconia or agate materials, mixing, drying and sieving by using a 120-mesh sieve to obtain a mixed raw material, wherein the rotating speed is 300r/min and the time is 4 h;
(3) placing the mixed raw materials in a high-temperature reaction furnace, and reacting for 2h at 1700 ℃ in the air atmosphere to obtain light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles;
(4) carrying out wet ball milling on the light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles, wherein the ball milling takes absolute ethyl alcohol as a medium, a ball milling tank and a milling ball are made of zirconia or agate materials, the rotating speed is 300r/min, the time is 4h, and the light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles are obtained by drying and sieving through a 120-mesh sieve after ball milling;
(5) cold press molding is carried out on the light-heavy rare earth mixed high-entropy rare earth silicate ceramic powder, the pressure of the cold press molding is 30MPa, and the pressure maintaining time is 1 min; then carrying out cold isostatic pressing, wherein the pressure of the cold isostatic pressing is 250MPa, and the pressure maintaining time is 10min, so as to obtain a light-heavy rare earth mixed high-entropy rare earth silicate block blank;
(6) placing the light and heavy rare earth mixed high-entropy rare earth silicate ceramic blocky blank into a high-temperature reaction furnace, sintering in the air atmosphere at 1750 ℃ for 2h to obtain a heavy rare earth mixed high-entropy rare earth silicate compact block (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5。
Prepared by this example (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5X-ray diffraction results, surface and fracture scanning electron microscope results and implementationExample 1 is consistent, and the compactness is more than 96%.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (4)
1. The light and heavy rare earth mixed high-entropy rare earth silicate compact block is characterized in that the chemical formula of the light and heavy rare earth mixed high-entropy rare earth silicate compact block is as follows: (Ho)0.25Lu0.25Yb0.25Eu0.25)2SiO5The preparation method of the light and heavy rare earth mixed high-entropy rare earth silicate compact block comprises the following steps:
s1, according to Ho2O3:Lu2O3:Yb2O3:Eu2O3:SiO2Weighing the raw materials according to the molar ratio of 1:1:1:1: 4;
s2, uniformly mixing the raw materials in the step S1 by adopting a wet mixing method, drying and sieving to obtain mixed raw materials;
s3, carrying out high-temperature reaction on the mixed raw materials in the step S2 to obtain light and heavy rare earth mixed high-entropy rare earth silicate ceramic particles, wherein the high-temperature reaction is carried out at 1500-1700 ℃ for 2-8h in an air atmosphere;
s4, carrying out wet ball milling on the heavy rare earth mixed high-entropy rare earth silicate ceramic particles obtained in the step S3, drying and sieving to obtain light rare earth mixed high-entropy rare earth silicate ceramic powder;
s5, carrying out cold press molding and cold isostatic pressing on the light and heavy rare earth mixed high-entropy rare earth silicate ceramic powder obtained in the step S4 to obtain a light and heavy rare earth mixed high-entropy rare earth silicate block blank, wherein the pressure of the cold press molding is 10-30MPa, and the pressure maintaining time is 1-5 min; the pressure of the cold isostatic pressing is 100-250MPa, and the pressure maintaining time is 10-30 min;
s6, performing high-temperature sintering on the light and heavy rare earth mixed high-entropy rare earth silicate block blank obtained in the step S5 in an air atmosphere to obtain a light and heavy rare earth mixed high-entropy rare earth silicate compact block, wherein the high-temperature sintering temperature is 1400-1750 ℃, and the heat preservation time is 2-12 h.
2. The dense block of light-heavy rare earth-mixed high-entropy rare earth silicate as claimed in claim 1, wherein in step S2, ethanol is used as a medium in the wet mixing, the rotation speed is 100-300r/min, and the time is 4-12 h.
3. The dense block of light and heavy rare earth mixed high-entropy rare earth silicate as claimed in claim 1, wherein the wet ball milling in step S4 uses ethanol as a medium, and the rotation speed is 100-300r/min and the time is 4-12 h.
4. The dense block of light-heavy rare earth-mixed high-entropy rare earth silicate in accordance with claim 1, wherein Ho is defined in step S12O3、Lu2O3、Yb2O3、Eu2O3、SiO2The purity of (A) is 99.9% -99.99%.
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