CN107698255B - Eu-Gd-Dy three rare earth ion tantalate and preparation method and application thereof - Google Patents
Eu-Gd-Dy three rare earth ion tantalate and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses Eu-Gd-Dy three rare earth ion tantalate and a preparation method and application thereof, wherein the Eu-Gd-Dy three rare earth ion tantalate has a chemical general formula of EuaGdbDycTaO7Wherein a + b + c is 3, and a, b and c are 0.8-1.2. The preparation method comprises the following steps: 1) europium chloride, gadolinium nitrate, dysprosium nitrate and tantalum oxalate are weighed according to the stoichiometric ratio, mechanically mixed with a set amount of citric acid under the condition of heat preservation, concentrated ammonia water is added in the mixing process to neutralize the solution, and then mechanical mixing is carried out under the condition of heat preservation to promote the reaction. 2) Drying the obtained solution, and then calcining at high temperature to remove carbon impurities to obtain Eu-Gd-Dy three rare earth ion tantalate powder. The Eu-Gd-Dy three rare earth ion tantalate has good high-temperature thermal stability and low thermal conductivity coefficient, and can be applied as a thermal barrier coating material.
Description
Technical Field
The invention relates to tantalate, in particular to Eu-Gd-Dy three rare earth ion tantalate and a preparation method and application thereof.
Background
With the development of aviation, aerospace and civil technologies, the requirement on the use temperature of hot end parts is higher and higher, and the limit condition of high-temperature alloys and single crystal materials is reached. Taking the heated components of the fuel turbine such as nozzles, vanes, combustors as examples, they are subjected to severe environments such as high temperature oxidation and high temperature gas stream erosion, and are subjected to temperatures as high as 1100 ℃, which exceed the limit temperature (1075 ℃) for high temperature nickel alloys. The thermal barrier coating prepared by combining the advantages of high strength and high toughness of metal and high temperature resistance of ceramic can solve the problems, has the functions of heat insulation, oxidation resistance and corrosion resistance, has a certain application on hot end materials such as steam turbines, diesel generators, jet engines and the like, and prolongs the service life of hot end parts.
Currently, the ceramic materials most suitable as thermal barrier coatings are mainly Yttria Stabilized Zirconia (YSZ), rare earth zirconates (RE)2Zr2O7) Rare earth silicates (RE)2SiO5) Rare Earth Phosphates (REPO)4) Rare earth cerates (RE)2Ce2O7) And rare earth stannates (RE)2Sn2O7) And the like. The most widely used is Yttria Stabilized Zirconia (YSZ), which has high melting point, low thermal conductivity, high thermal expansion coefficient and good mechanical properties, but the use temperature is low, only 1200 ℃, because YSZ undergoes phase change at over 1200 ℃ to cause volume change, so that the coating fails. In addition to YSZ, the currently used thermal barrier coating material is La2Zr2O7The rare earth zirconate has lower thermal conductivity compared with YSZ, and the using temperature is as high as 1600 ℃, because the rare earth zirconate is a pyrochlore and defect fluorite type structure, has a large amount of crystal defects and can effectively scatter phonons, thereby reducing the thermal conductivity, and has no phase change and other problems at high temperature. Therefore, when a novel thermal barrier coating material is searched, a low-thermal-conductivity material with good high-temperature phase stability can be searched from a crystal structure.
Rare earth tantalate RE3TaO7Is a novel thermal barrier coating material, and studies by Yoshiyuki et al show (Yoshiyuki Yokogawa, Masahiro Yoshimura and Shigeyuki Somiya; Order-recorder in R3TaO7(R: rare earth) drugs, Solid State ionics:28-30(1988)1250-1253) in RE3TaO7The ordered-disordered change from pyrochlore to defect fluorite structure conversion occurs along with the change of the radius of the rare earth ions, and the ordered-disordered change is related with rare earth zirconate (RE)2Zr2O7) Similarly. It can therefore be surmised that two oxide ceramics having similar crystal structures may have the same characteristics, such as high melting point, low thermal conductivity, high coefficient of thermal expansion and the like,moreover, the results of previous studies show that RE is a very important element in the field of radio communications3TaO7Is a ferroelastic material, which is the same as YSZ, and thus has good mechanical properties at high temperatures.
Disclosure of Invention
The invention aims to provide Eu-Gd-Dy three rare earth ion tantalate with low thermal conductivity and good thermal stability as well as a preparation method and application thereof.
To achieve the purpose, the Eu-Gd-Dy three rare earth ion tantalite provided by the invention has the chemical general formula of EuaGdbDycTaO7Wherein a + b + c is 3, and a, b and c are 0.8-1.2. Preferably, a ═ b ═ c ═ 1, in this case, the chemical formula of the Eu-Gd-Dy three rare earth ion tantalate is EuGdDyTaO7。
Preferably, the Eu-Gd-Dy three rare earth ion tantalate has the following properties: 1) the average grain size is 2-10 μm; 2) the thermal conductivity is 1.4-1.8 W.m at the temperature of 100-800 DEG C-1·K-1And decreases with increasing temperature; 3) in the XRD pattern, the angles at which diffraction peaks are arranged in a descending manner according to relative intensity are as follows: 30 +/-1 degrees, 49 +/-1 degrees, 34.5 +/-1 degrees, 58 +/-1 degrees and 61 +/-1 degrees.
The invention also provides a preparation method of the Eu-Gd-Dy three rare earth ion tantalate, which comprises the following steps:
1) weighing europium chloride, gadolinium nitrate, dysprosium nitrate and tantalum oxalate according to a stoichiometric ratio, mechanically mixing the europium chloride, gadolinium nitrate, dysprosium nitrate and tantalum oxalate with a set amount of citric acid under a heat preservation condition, adding concentrated ammonia water to neutralize the solution in the mixing process, and mechanically mixing the solution under the heat preservation condition to promote chemical reaction:
in the reaction, the sum of the substances of the three rare earth elements, tantalum oxalate and citric acid is 6: 1: 8, and the amount of each rare earth element substance is determined according to a stoichiometric coefficient; the citric acid can then be calcined out and therefore can be in slight excess; the amount of ammonia added is preferably such that the solution is near neutral.
2) Drying the obtained solution, and then calcining at high temperature to remove carbon impurities to obtain Eu-Gd-Dy three rare earth ion tantalate powder.
Preferably, in the step 1), the temperature is 135 +/-10 ℃ and the time is 50 +/-10 min during the first mechanical mixing; the second mechanical mixing is carried out at 180 + -20 deg.C for 30 + -10 min.
Preferably, in the step 2), the drying temperature is 300 +/-10 ℃, and the drying time is 10 +/-1 h; the calcining temperature is 800 +/-10 ℃, and the calcining time is 10 +/-1 h.
The Eu-Gd-Dy three rare earth ion tantalate has low thermal conductivity and high thermal expansion coefficient, and can be used as a thermal barrier coating material. One application mode of the material as a thermal barrier coating material is as follows: and (3) sending the Eu-Gd-Dy three rare earth ion tantalate into atmospheric plasma spraying equipment in a powder form, and carrying out atmospheric plasma spraying on the surface of the substrate to prepare the high-temperature thermal barrier coating. Atmospheric Plasma Spray (APS) and electron beam-physical vapor deposition (EB-PVD) are the predominant methods currently used to prepare thermal barrier coatings. Compared with the atmospheric plasma spraying, the EB-PVD thermal barrier coating has lower deposition efficiency, uncontrollable coating thickness, complex surface cleaning, complex and expensive equipment, relatively lower deposition rate, complex process flow and small sample size, so the high-temperature ceramic coating is prepared by adopting the atmospheric plasma spraying mode.
Preferably, the Eu-Gd-Dy three rare earth ion tantalate is granulated and then sent into atmospheric plasma spraying equipment for spraying; the granulating step comprises: 1) mixing a binder into the Eu-Gd-Dy three rare earth ion tantalate powder to prepare a muddy liquid, 2) sending the muddy liquid into a spray dryer to spray to prepare spherical granulated powder, and sieving the spherical granulated powder to obtain powder with the particle size of 40-50 mu m. The binder is preferably a high-viscosity agar solution with the viscosity of 900-1200 MPa & S.
Preferably, when the atmospheric plasma spraying is carried out, Ar and He are used as ion gases, the flow rate of the Ar gas is 50-100L/min, and the flow rate of the He gas is 6-20L/min; the arc voltage is 50-80V, and the arc current is 500-800A; the powder feeding speed is 20-110 g/min, the powder feeding angle is 60-90 degrees, and the spraying distance is 90-130 mm.
The invention has the following beneficial effects:
1) the Eu-Gd-Dy three rare earth ion tantalate EuaGdbDycTaO7Can obtain rare earth tantalate RE compared with the prior art3TaO7Better thermal properties such as better high temperature thermal stability (no phase change at 1600 ℃), lower thermal conductivity and higher thermal expansion coefficient (-12.8 x 10)-6K-11200 ℃), can effectively reduce the thermal mismatch with the alloy matrix. Compared with double rare earth ion tantalates (patent application number: CN201610597143.4), the Eu-Gd-Dy triple rare earth ion tantalates in the invention are of a defect fluorite crystal structure, have high oxygen vacancy concentration, can effectively reduce the thermal conductivity, and have no phase change at high temperature; the double rare earth ion tantalite is of a monoclinic phase (m) structure, and has m-t phase change at high temperature, large volume change and the like, which can cause failure of a coating in practical application.
2) The preparation method adopts a liquid phase reaction system, fully mixes the three rare earth ions, and promotes the full reaction between the raw materials through heat preservation mechanical mixing and the addition of concentrated ammonia water. With citric acid and ammonia, impurities can be removed by reaction and calcination, with other acids or alkaline solutions, producing impurities in the product that are difficult to remove. The prepared Eu-Gd-Dy three rare earth ion tantalate has high purity, less impurity content, high density, small crystal grain size, less defects such as air holes, cracks and the like, and has good mechanical properties.
3) The Eu-Gd-Dy three rare earth ion tantalate is tested, and the result shows that the grain size is 2-10 mu m; the thermal conductivity is 1.4-1.8 W.m at the temperature of 100-800 DEG C-1·K-1And decreases with increasing temperature; in the XRD pattern, the angles at which diffraction peaks are arranged in a descending manner according to relative intensity are as follows: 30 +/-1 degrees, 49 +/-1 degrees, 34.5 +/-1 degrees, 58 +/-1 degrees and 61 +/-1 degrees.
5) The Eu-Gd-Dy three rare earth ion tantalate has good high-temperature phase stability, high hardness, low thermal conductivity and high thermal expansion coefficient, is used as a novel thermal barrier coating material, and has a good thermal insulation effect.
Drawings
FIG. 1 is the Eu-Gd-Dy three rare earth ion tantalate EuGdDyTaO provided in example 17X-ray diffraction pattern (XRD pattern) of the high-temperature ceramic block of (a);
FIG. 2 is the Eu-Gd-Dy three rare earth ion tantalate EuGdDyTaO provided in example 17The picture of the high-temperature ceramic block of (1);
FIG. 3 is the Eu-Gd-Dy three rare earth ion tantalate EuGdDyTaO provided in example 17Scanning Electron Microscope (SEM) of the high temperature ceramic block of (a);
FIG. 4 is the Eu-Gd-Dy three rare earth ion tantalate EuGdDyTaO provided in example 17The thermal conductivity of the high-temperature ceramic block is the same as that of yttria-stabilized zirconia (7YSZ) and rare earth zirconate (La)2Zr2O7) And europium tantalate (Eu)3TaO7) Compare the figures.
Detailed Description
The present invention will be described in further detail with reference to the drawings and embodiments 1 to 7.
The chemical general formula of the Eu-Gd-Dy three rare earth ion tantalate provided by the invention is EuaGdbDycTaO7Wherein a + b + c is 3, and a, b and c are 0.8-1.2. In each example, the coefficients of Eu, Gd, and Dy are shown in Table 1.
The preparation method of the Eu-Gd-Dy three rare earth ion tantalate comprises the following steps:
(1) weighing europium chloride (EuCl) according to stoichiometric ratio3) Gadolinium nitrate (Gd (NO)3)3) Dysprosium nitrate (Dy (NO)3)3) And tantalum oxalate (Ta)2(C2O4)5) Adding citric acid (C)6H8O7) The specific amounts of the additives in the examples are shown in Table 1 (the amounts are converted into mass when weighing, and the amounts are measured in moles for the convenience of indicating the stoichiometric ratio in the present invention). Keeping the temperature at 135 ℃ for 50min, carrying out violent mechanical stirring to fully mix the components, dripping concentrated ammonia water neutralizing solution at the speed of 1mL/min in the stirring process (the temperature is kept for 50min according to the temperature keeping time,dropwise added to neutrality), followed by incubation at 180 ℃ for 30min and vigorous mechanical stirring to facilitate the reaction.
2) The resulting solution was heated to 300 ℃ and allowed to warm for 10 hours to dry. And placing the obtained solid powder in a sintering furnace, heating to 800 ℃, and preserving heat for 10 hours to perform decarbonization treatment.
3) Tabletting the powder obtained in the step 2). And (3) maintaining the pressure for 2min at 4MPa, and finally sintering at 1680 ℃ for 8 hours to obtain a compact Eu-Gd-Dy three rare earth ion tantalate ceramic block, wherein the picture of the compact Eu-Gd-Dy three rare earth ion tantalate ceramic block is shown in figure 2, so that the block surface has no pores or cracks and has good surface quality.
Table 1 raw material ratios and test data for each example
4) The obtained ceramic bulk was subjected to X-ray diffraction, and EuGdDyTaO obtained in example 1 was shown in FIG. 17The XRD spectrum of the block body has the diffraction peaks at the angles of descending arrangement according to the relative intensity: 30 +/-1 degrees, 49 +/-1 degrees, 34.5 +/-1 degrees, 58 +/-1 degrees and 61 +/-1 degrees. The XRD patterns of other examples were substantially the same as those of example 1, and only part of the diffraction peaks were different in intensity. And Dy3TaO7The standard PDF card PDF Number of (1): 38-1406, the diffraction peaks displayed by the compact ceramic X-ray diffraction result of Eu-Gd-Dy three rare earth ion tantalate are consistent with the number of standard PDF cards and are in one-to-one correspondence with the standard PDF cards, which shows that the crystal structure type of the prepared sample is consistent with that of the standard cards and no impurity phase exists. The phase of the obtained sample is orthogonal, the included angles of three axes abc in the crystal structure are all 90 degrees, the lengths of a, b and C in the crystal structure are different, and the space point group is C2221. Furthermore, all diffraction peaks of the obtained samples are shifted to the right from the standard card due to the doped rare earth ion Eu3 +、Gd3+Has a specific ratio of Dy3+The larger ion radius increases the average radius of the rare earth ions, resulting in an increase in the lattice constant and an extension of the atomic distance.
5) The ceramic blocks obtained in each example were photographed by a Scanning Electron Microscope (SEM), and EuGdDyTaO obtained in example 1 is shown in FIG. 37As can be seen from the SEM picture of the block, the prepared Eu-Gd-Dy three rare earth ion tantalate ceramic has a compact structure, fine crystal grains (2-5 mu m), no cracks and only trace pores, and the test result shows that the compactness of the Eu-Gd-Dy three rare earth ion tantalate ceramic reaches 94%. The average grain size ranges measured for each example are detailed in table 1.
6) EuGdDyTaO obtained in example 1 was continuously measured by a laser reflectance method (LFA 457)7The block body has thermal conductivity at 100-800 ℃, the result is plotted in figure 4, and the thermal barrier coating materials 7YSZ and La which are widely applied at present are given as a comparison figure2Zr2O7And Eu3TaO7Thermal conductivity of (2). As can be seen from FIG. 1, EuGdDyTaO prepared in example 17The block body has a thermal conductivity of 1.4-1.7 W.m at a temperature of 100-800 DEG C-1·K-1Far below 7YSZ and La2Zr2O7And Eu3TaO7The thermal insulation effect is used as the main function of the thermal barrier coating, and the low thermal conductivity is the most critical performance, so that the SmEuGdTaO7 ceramic can be popularized and applied as a thermal barrier coating material. The range of thermal conductivities measured for each example is detailed in table 1, with the smaller being 100 ℃ measurements and the larger being 800 ℃.
An application example of the Eu-Gd-Dy three rare earth ion tantalate is given below.
In the application example, Eu-Gd-Dy three rare earth ion tantalite is sprayed on the surface of a nickel-based alloy steel matrix by adopting atmospheric plasma spraying, and the method comprises the following specific steps:
1) adding Eu-Gd-Dy three rare earth ion tantalate powder obtained in the preparation step 2) into a high-viscosity agar solution with the sol viscosity of 1200 MPa.S when the concentration is 2%, keeping the temperature around 60 ℃, and stirring to prepare a muddy liquid.
2) Spraying the slurry liquid by a spray dryer with 25000rpm, inlet temperature of 160 ℃ and outlet temperature of 78 ℃ to prepare spherical granulation powder with the particle size of 30-60 mu m.
3) Then grinding the spherical granulation powder (if necessary, the prepared powder can be directly sieved if the particle size is proper), then placing the powder on sieves which are vertically placed at the upper and lower parts of 50 mu m and 40 mu m for sieving, and taking the powder in the middle to obtain particles of 40-50 mu m.
4) Spraying was carried out using an atmospheric plasma spraying apparatus (Sluzer metco Unicoat) spray gun type 9 MB. The spraying gas environment is Ar/He: the Ar flow rate is 80L/min, and the He flow rate is 12L/min; the arc voltage is 80V, the arc current is 500A, the powder feeding speed is 110g/min, the powder feeding angle is 90 degrees, and the spraying distance is 130 mm. In the spraying process, a circulating water cooling method is adopted to cool the matrix, and the flow rate of cooling water flow is 200L/min. Cooling to room temperature to obtain the required high-temperature ceramic thermal barrier coating (thermal conductivity: 1.4-1.8 W.m.)-1.K-1)。
Claims (9)
1. A Eu-Gd-Dy three rare earth ion tantalate is characterized in that: the chemical general formula of the tantalate is EuaGdbDycTaO7Wherein a + b + c is 3, and a, b and c are 0.8-1.2; and the crystal structure of the tantalate is defect fluorite type and has the following properties: 1) the grain size is 2-10 μm; 2) the thermal conductivity is 1.4-1.8 W.m at the temperature of 100-800 DEG C-1·K-1And decreases with increasing temperature; 3) in the XRD pattern, the angles at which diffraction peaks are arranged in a descending manner according to relative intensity are as follows: 30 +/-1 degrees, 49 +/-1 degrees, 34.5 +/-1 degrees, 58 +/-1 degrees and 61 +/-1 degrees.
2. The Eu-Gd-Dy three rare earth ion tantalate of claim 1, wherein: a, b, c, 1.
3. A method for preparing Eu-Gd-Dy tri-rare earth ion tantalate according to claim 1 or 2, characterized in that: the method comprises the following steps:
1) weighing europium chloride, gadolinium nitrate, dysprosium nitrate and tantalum oxalate according to a stoichiometric ratio, mechanically mixing the europium chloride, gadolinium nitrate, dysprosium nitrate and tantalum oxalate with a set amount of citric acid under a heat preservation condition, adding concentrated ammonia water to neutralize the solution in the mixing process, and mechanically mixing the solution under the heat preservation condition to promote the chemical reaction;
2) drying the obtained solution, and then calcining at high temperature to remove carbon impurities to obtain Eu-Gd-Dy three rare earth ion tantalate.
4. The method for preparing Eu-Gd-Dy three rare earth ion tantalate according to claim 3, wherein: in the step 1), the temperature is 135 +/-10 ℃ and the time is 50 +/-10 min during the first mechanical mixing; the temperature is 180 + -20 deg.C and the time is 30 + -10 min during the second mechanical mixing; in the step 2), the drying temperature is 300 +/-10 ℃, and the drying time is 10 +/-1 h; the calcining temperature is 800 +/-10 ℃, and the calcining time is 10 +/-1 h.
5. The method for preparing Eu-Gd-Dy three rare earth ion tantalate according to claim 3, wherein: in the step 1), the sum of the contents of the three rare earth elements, tantalum oxalate and citric acid is 6: 1: 8.
6. Use of Eu-Gd-Dy tri-rare earth ion tantalate as defined in any one of claims 1 to 2 as a thermal barrier coating material.
7. The use of Eu-Gd-Dy tri-rare earth ion tantalate as defined in claim 6 as a thermal barrier coating material, wherein: and (3) sending the Eu-Gd-Dy three rare earth ion tantalate into atmospheric plasma spraying equipment in a powder form, and carrying out atmospheric plasma spraying on the surface of the substrate to prepare the thermal barrier coating with low thermal conductivity and high thermal expansion coefficient.
8. The use of Eu-Gd-Dy tri-rare earth ion tantalate as defined in claim 7 as a thermal barrier coating material, wherein: granulating the Eu-Gd-Dy three rare earth ion tantalate, and then sending the granules into atmospheric plasma spraying equipment for spraying; the granulating step comprises: 1) mixing a binder into the Eu-Gd-Dy three rare earth ion tantalate powder to prepare a muddy liquid, 2) sending the muddy liquid into a spray dryer to spray to prepare spherical granulated powder, and sieving the spherical granulated powder to obtain powder with the particle size of 40-50 mu m.
9. Use of Eu-Gd-Dy tri-rare earth ion tantalate according to claim 7 or 8 as a thermal barrier coating material, characterized in that: when the atmospheric plasma spraying is carried out, Ar and He are used as ion gases, the flow rate of the Ar gas is 50-100L/min, and the flow rate of the He gas is 6-20L/min; the arc voltage is 50-80V, and the arc current is 500-800A; the powder feeding speed is 20-110 g/min, the powder feeding angle is 60-90 degrees, and the spraying distance is 90-130 mm.
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| JP2012176883A (en) * | 2011-01-31 | 2012-09-13 | Canon Inc | Composition for optical member, and the optical member |
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| CN106278260A (en) * | 2016-07-27 | 2017-01-04 | 昆明理工大学 | A kind of preparation method of pair of rare earth ion tantalates high-temperature ceramics |
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| CN106278260A (en) * | 2016-07-27 | 2017-01-04 | 昆明理工大学 | A kind of preparation method of pair of rare earth ion tantalates high-temperature ceramics |
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