CN113562765B - Preparation of high-entropy rare earth tantalate RETaO by molten salt method 4 Method for preparing spherical powder - Google Patents
Preparation of high-entropy rare earth tantalate RETaO by molten salt method 4 Method for preparing spherical powder Download PDFInfo
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Abstract
The invention discloses a method for preparing high-entropy rare earth tantalate RETaO by a molten salt growth method 4 The method of spherical powder, wherein RE is at least one of yttrium, aluminum and lanthanide rare earth elements. The preparation method of the rare earth tantalate spherical powder comprises the following steps of 2 O 3 And Ta 2 O 5 Mixing the mixture with equimolar mixture, adding the mixture and KCl and NaCl mixed molten salt into a ball mill for ball milling, drying, sieving, calcining, cooling, cleaning, filtering, drying for the second time, and sieving to obtain the finished product. The method has the advantages of low synthesis temperature, short reaction time, simple process, high purity of synthesized products, high sphericity rate, good fluidity, controllable crystal form and morphology of powder particles, no agglomeration, easy dispersion and the like.
Description
1.1.1 technical field
The invention relates to the technical field of ceramic powder preparation, and particularly relates to a method for preparing high-entropy rare earth tantalate (RETaO) by using a molten salt growth method 4 A method for preparing spherical powder.
1.1.2 background Art
In recent years, "high entropy" has become a hot direction in the field of material research, i.e., the development of new materials with superior properties by introducing structural entropy. Based on four high entropy effects: (1) the thermodynamic high entropy effect; (2) the effect of lattice distortion; (3) a hysteresis diffusion effect; (4) the 'mixing effect' of the multi-principal element shows excellent properties such as high strength, high toughness, corrosion resistance, wear resistance, excellent thermal property, excellent electrical property and the like, so that the 'high entropy' can obviously improve the comprehensive properties of the material.
The high-entropy ceramics have the advantages of high melting point, high hardness, high toughness, low thermal conductivity, corrosion resistance and the like, and show great development potential in the field of Thermal Barrier Coatings (TBCs). Wang et al use the high entropy Effect on RETaO 4 The comprehensive performance of the ceramics is optimized, and the (5 RE) is systematically researched 0.2 )TaO 4 The phase structure, the ferroelastic toughening mechanism, the thermal property and the mechanical property of the (5 RE) 0.2 )TaO 4 Has great application potential in TBCs. Tangan powder and the like are used for preparing yttria-stabilized zirconia (YSZ) hollow sphere powder serving as a thermal barrier coating material, and the comprehensive performance of the yttria-stabilized zirconia (YSZ) hollow sphere powder is improved to a certain extent. The preparation of rare earth tantalate thermal barrier coating powders is a very critical step in the preparation of TBCs, and its quality directly affects the performance of the coating. Chinese patent CN109627000A discloses a rare earth tantalum/niobate (RETa/NbO) 4 ) The ceramic powder and the preparation method thereof have the problems of low powder purity, high synthesis temperature, loss in the centrifugal spray granulation process and the like in the calcination process.
1.1.3 summary of the invention
In view of this, the invention aims to provide a molten salt method for preparing high-entropy rare earth tantalate RETaO 4 Method for preparing rare earth tantalate RETaO with high purity, high sphericity and good fluidity from spherical powder 4 Spherical powder.
In order to achieve the purpose, the invention provides the following technical scheme:
1. high-entropy rare earth tantalate RETaO prepared by molten salt method 4 The method for preparing spherical powder is characterized by comprising the following steps:
(1) weighing raw materials and molten salt, taking absolute ethyl alcohol as a medium, and carrying out ball milling uniformly in a ball mill;
(2) drying and sieving the product obtained in the step (1), and then heating and calcining;
(3) cooling and cleaning the product obtained in the step (2);
(4) filtering, secondary drying and sieving the powder washed in the step (3) to obtain the powder;
the rare earth tantalate RETaO 4 In the formula (II), RE is at least one of yttrium, aluminum and lanthanide rare earth elements.
The raw material is RE 2 O 3 And Ta 2 O 5 Said RE 2 O 3 Is Y 2 O 3 、Al 2 O 3 、La 2 O 3 、Ce 2 O 3 、Nd 2 O 3 、Pm 2 O 3 、Sm 2 O 3 、Eu 2 O 3 、Gd 2 O 3 、Tb 2 O 3 、Dy 2 O 3 、Ho 2 O 3 、Er 2 O 3 、Tm 2 O 3 、Yb 2 O 3 、Lu 2 O 3 At least one of;
the molten salt is a mixed salt of KCl and NaCl.
Preferred in the present invention, the raw material RE in the step (1) 2 O 3 And Ta 2 O 5 In a molar ratio of 1: 1, purity of the starting Material>99.99 percent and the grain diameter is 1-80 mu m.
In the invention, preferably, in the step (1), the purity of the molten salt is more than 99.99%, the particle size is 1-80 μm, and the mass ratio of KCl to NaCl is (1-5): (1-2), the mass ratio of the raw materials to the molten salt is (1-2): (1-7).
Further preferably, in the invention, the mass ratio of the molten salt KCl to NaCl in the step (1) is optimized to be 5:1, optimizing the mass ratio of the raw materials to the molten salt to be 1: 6.
in the invention, the rotation speed of the ball milling in the step (1) is preferably 350r/min, and the ball milling time is preferably 12 h.
In the present invention, preferably, the drying in step (2) is drying at 90 ℃ for 24 hours, and the sieving is 400-mesh sieving.
In the invention, preferably, the calcining temperature in the step (2) is 600-1200 ℃, the time is 4-8h, and the heating rate is 5-10 ℃/min.
In the present invention, it is further preferred that the calcination temperature in step (2) is 800 ℃ and the calcination time is 6 hours.
In the invention, preferably, in the step (4), the drying is carried out at 90 ℃ for 24h, and the sieving is carried out by sieving with a 100-mesh sieve and then sieving with a 400-mesh sieve.
2. High-entropy rare earth tantalate RETaO prepared by the method 4 Spherical powder.
The invention has the beneficial effects that:
1. rare earth tantalate synthesized by molten salt method 4 The spherical powder has high purity and low synthesis temperature.
2. The method of the invention can be controlledThe proportion of the fused salt to the raw material, the fused salt components, the calcination temperature and the calcination time are used for controlling the morphology and the particle size of the powder, so as to obtain the rare earth tantalate RETaO with high sphericity rate and good fluidity 4 Spherical powder.
3. The rare earth tantalate RETaO prepared by the invention 4 The spherical powder has the characteristics of uniform particle size, excellent performance, stable quality, strong controllability, suitability for industrial production and the like.
1.1.4 description of the drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 shows the preparation of (Y) by the molten salt method in example 1 0.2 Ce 0.2 Sm 0.2 Gd 0.2 Dy 0.2 )TaO 4 An XRD pattern of (a);
FIG. 2 shows the preparation of (Y) by the molten salt method in example 1 0.2 Ce 0.2 Sm 0.2 Gd 0.2 Dy 0.2 )TaO 4 SEM spectrum of (d).
1.1.5 detailed description
The present invention is further described with reference to the following drawings and specific examples so that those skilled in the art can better understand the present invention and can practice the present invention, but the examples are not intended to limit the present invention.
Example 1
In this example, a molten salt method is used to prepare high-entropy rare earth tantalate (Y) 0.2 Ce 0.2 Sm 0.2 Gd 0.2 Dy 0.2 )TaO 4 The method for preparing the spherical powder comprises the following steps:
according to 1/5: 1/5: 1/5: 1/5: 1/5: 1 molar ratio of Y 2 O 3 、Ce 2 O 3 、Sm 2 O 3 、Gd 2 O 3 、Dy 2 O 3 And Ta 2 O 5 Total 5kg, purity of raw material and molten salt>99.99%, the particle diameter is 1-80 μm, and the ratio of (1-5): (1-2) weighing a mixed salt of KCl and NaCl according to the proportion shown in Table 1, and mixing the KCl and NaCl according to the proportion of 1: 3 weighing raw materials and molten salt, pouring the raw materials and the molten salt into a ball milling tank, and ball milling the raw materials and the molten salt for 12 hours (350 r/m) in a planetary ball mill by taking absolute ethyl alcohol as a mediumin), the chemical reaction formula of the raw material is: RE 2 O 3 +Ta 2 O 5 ＝2RETaO 4 . Drying the reacted product at 90 deg.C for 24 hr, sieving with 400 mesh sieve, calcining in resistance furnace at 1000 deg.C and 6 hr respectively at a heating rate of 5 deg.C/min, cooling with the furnace after calcination, taking out the powder when the temperature is reduced to room temperature, repeatedly washing the obtained product with heated deionized water for several times to remove excessive chloride salt until silver nitrate (AgNO) is used 3 ) Reagent test filtrate does not contain Cl - Filtering the washed powder, drying at 90 ℃ for 24 hours, sieving with a 100-mesh sieve, sieving with a 400-mesh sieve, testing the particle size of the powder by using a laser particle sizer, testing the flowability by using a Hall flow meter, observing the morphology of the powder particles by using a scanning electron microscope, and calculating the sphericity ratio.
FIG. 1 is an XRD pattern of high-entropy rare earth tantalate synthesized by molten salt method, which is compared with a single-phase PDF standard card, GdTaO 4 (PDF: 24-0441) and DyTaO 4 (PDF: 12-0379) peaks were slightly shifted in position due to lattice distortion of crystal structure caused by high entropy effect, peak shift caused by increase in defect concentration, etc., and high entropy rare earth tantalate (Y) was found by comparison with a single phase standard card 0.2 Ce 0.2 Sm 0.2 Gd 0.2 Dy 0.2 )TaO 4 The purity is high. As shown in FIG. 2, the observation (Y) was carried out by a Scanning Electron Microscope (SEM) 0.2 Ce 0.2 Sm 0.2 Gd 0.2 Dy 0.2 )TaO 4 The microscopic morphology and sphericity ratio of the spherical powder show that the particle size is 40-90 μm, and the sphericity ratio>99%, it is clear from Table 1 that KCl and NaCl in a ratio of 5:1 have a good sphericity ratio and fluidity.
TABLE 1 ratio of KCl and NaCl in molten salt to rare earth tantalate (Y) 0.2 Ce 0.2 Sm 0.2 Gd 0.2 Dy 0.2 )TaO 4 Relationship between sphericity and fluidity
Example 2
In this example, a molten salt method is used to prepare high-entropy rare earth tantalate (Lu) 1/3 Pm 1/3 Eu 1/3 )TaO 4 The method for preparing the spherical powder comprises the following steps:
according to 1/3: 1/3: 1/3: weighing Lu at a molar ratio of 1 2 O 3 、Pm 2 O 3 、Eu 2 O 3 And Ta 2 O 5 5kg in total, according to the weight ratio of 5:1 proportion weighing KCl and NaCl mixed salt, raw material and molten salt purity>99.99%, the particle size is 1-80 μm, and the mass ratio (1-2): (2-7) weighing raw materials and molten salt, pouring the raw materials and the molten salt into a ball milling tank, as shown in table 2, ball milling the raw materials and the molten salt for 12h (350r/min) in a planetary ball mill by using absolute ethyl alcohol as a medium, drying the raw materials at 90 ℃ for 24h, sieving the raw materials by using a 400-mesh sieve, then placing the raw materials into a resistance furnace for calcination, wherein the calcination temperature and the calcination time are 900 ℃ and 6h respectively, the heating rate is 5 ℃/min, cooling the raw materials with the furnace after the calcination is finished, taking out the powder after the temperature is reduced to the room temperature, repeatedly washing the obtained product by using heated deionized water for several times to remove redundant chloride salt until silver nitrate (AgNO) is used 3 ) Reagent test filtrate does not contain Cl - The washed powder was filtered, dried at 90 ℃ for 24 hours, sieved first with 100 mesh and then with 400 mesh, the particle size of the powder was measured with a laser particle sizer, the flowability was measured with a hall flow meter, and the ratio of raw material to molten salt was found to be 1: (5-7), the powder has better sphericity rate and fluidity.
TABLE 2 raw materials and molten salt ratio and rare earth tantalate (Lu) 1/3 Pm 1/3 Eu 1/3 )TaO 4 Relationship between sphericity and fluidity
Example 3
In this example, a molten salt method is used to prepare high-entropy rare earth tantalate (Y) 1/4 Al 1/4 Sm 1/4 Er 1/4 )TaO 4 The method for preparing the spherical powder comprises the following steps:
according to 1/4: 1/4: 1/4: 1/4: 1 molar ratio of Y 2 O 3 、Al 2 O 3 、Sm 2 O 3 、Er 2 O 3 And Ta 2 O 5 5kg in total, according to the weight ratio of 5:1 proportion weighing KCl and NaCl mixed salt, raw material and molten salt purity>99.99%, the particle size is 1-80 μm, and the mass ratio is 1: 6 weighing raw materials and molten salt, pouring the raw materials and the molten salt into a ball milling tank, ball milling the raw materials and the molten salt for 12 hours (350r/min) in a planetary ball mill by using absolute ethyl alcohol as a medium, drying the raw materials for 24 hours at 90 ℃, sieving the raw materials by a 400-mesh sieve, then placing the raw materials into a resistance furnace for calcination, wherein the calcination temperature and the calcination time are respectively (600-1200 ℃) and 6 hours, the heating rate is 5 ℃/min, cooling the raw materials along with the furnace after the calcination is finished, taking out powder after the temperature is reduced to the room temperature, repeatedly washing the obtained product by using heated deionized water for several times to remove redundant chloride salt until silver nitrate (AgNO) is used 3 ) Reagent test filtrate does not contain Cl - The washed powder was filtered, dried at 90 ℃ for 24 hours, passed through 100 mesh sieve and then 400 mesh sieve, the particle size of the powder was measured by a laser particle sizer, the particle size was in the range of 40 μm to 90 μm, and the fluidity was measured by a Hall flow meter, and the fluidity was (32-97s)/50g, and it was found from the data in Table 3 that the powder had a good sphericity ratio and fluidity at a calcination temperature of 600 ℃ and 1000 ℃.
TABLE 3 calcination temperature and rare earth tantalates (Y) 1/4 Al 1/4 Sm 1/4 Er 1/4 )TaO 4 Relationship between sphericity and fluidity
Example 4
In this example, a molten salt method is used to prepare high-entropy rare earth tantalate (Er) 1/6 Sm 1/6 Pm 1/6 Nd 1/6 Yb 1/6 Eu 1/6 )TaO 4 The method for preparing the spherical powder comprises the following steps:
according to 1/6: 1/6: 1/6: 1/6: 1/6: 1/6: 1 molar ratio and Er weighing 2 O 3 、Sm 2 O 3 、Pm 2 O 3 、Nd 2 O 3 、Yb 2 O 3 、 Eu 2 O 3 And Ta 2 O 5 5kg in total, according to the weight ratio of 5:1 proportion weighing KCl and NaCl mixed salt, raw material and molten salt purity>99.99%, the particle size is 1-80 μm, and the mass ratio is 1: 6 weighing raw materials and molten salt, pouring the raw materials and the molten salt into a ball milling tank, ball milling the raw materials and the molten salt for 12h (350r/min) in a planetary ball mill by using absolute ethyl alcohol as a medium, drying the raw materials for 24h at 90 ℃, sieving the raw materials by a 400-mesh sieve, then placing the raw materials into a resistance furnace for calcination, wherein the calcination temperature and the calcination time are respectively 900 ℃ and (1-10h), the heating rate is 5 ℃/min, cooling the raw materials along with the furnace after the calcination is finished, taking out the powder body after the temperature is reduced to the room temperature, repeatedly washing the obtained product by heated deionized water for several times to remove the redundant chloride salt until silver nitrate (AgNO) is used 3 ) Reagent test filtrate does not contain Cl - The washed powder was filtered, dried at 90 ℃ for 24 hours, and sieved first through 100 mesh and then through 400 mesh.
High-entropy rare earth tantalate (Er) prepared by the scheme 1/6 Sm 1/6 Pm 1/6 Nd 1/6 Yb 1/6 Eu 1/6 )TaO 4 The spherical powder has better sphericity ratio and fluidity, and the grain size is increased along with the extension of sintering time. Please supplement the graph or table of the relationship between the sintering time (1-10h) and the grain size, the best effect is highlighted by 4-8 h.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (8)
1. Preparation of high-entropy rare earth tantalate RETaO by molten salt method 4 The method for preparing spherical powder is characterized by comprising the following steps:
(1) weighing raw materials and molten salt, taking absolute ethyl alcohol as a medium, and carrying out ball milling uniformly in a ball mill;
(2) drying and sieving the product obtained in the step (1), and then heating and calcining; calcining at 600-800 ℃ for 4-8h at a heating rate of 5 ℃/min;
(3) cooling and cleaning the product obtained in the step (2);
(4) filtering, secondary drying and sieving the powder washed in the step (3) to obtain the high-entropy rare earth tantalate RETaO 4 Spherical powder;
the rare earth tantalate RETaO 4 In the formula (II), RE is at least one of yttrium and lanthanide rare earth elements;
the raw material is RE 2 O 3 And Ta 2 O 5 Said RE 2 O 3 Is Y 2 O 3 、La 2 O 3 、Ce 2 O 3 、Nd 2 O 3 、Pm 2 O 3 、Sm 2 O 3 、Eu 2 O 3 、Gd 2 O 3 、Tb 2 O 3 、Dy 2 O 3 、Ho 2 O 3 、Er 2 O 3 、Tm 2 O 3 、Yb 2 O 3 、Lu 2 O 3 At least one of (a);
the molten salt is a mixed salt of KCl and NaCl, the purity of the molten salt is more than 99.99%, the particle size is 1-80 mu m, the mass ratio of KCl to NaCl is 5:1, and the mass ratio of the raw materials to the molten salt is 1: 5-7.
2. The molten salt method for preparing high-entropy rare earth tantalate (RETaO) according to claim 1 4 The method for preparing spherical powder is characterized by comprising the following steps: raw material RE in step (1) 2 O 3 And Ta 2 O 5 In a molar ratio of 1: 1, purity of the starting Material>99.99%, the particle size is 1-80 mu m.
3. The molten salt method for preparing high-entropy rare earth tantalate (RETaO) according to claim 1 4 The method for preparing spherical powder is characterized by comprising the following steps: in the step (1), the mass ratio of the molten salt KCl to NaCl is 5:1, the mass ratio of the raw materials to the molten salt is 1: 6.
4. the molten salt method for preparing high-entropy rare earth tantalum according to claim 1Acid salt RETaO 4 The method for preparing spherical powder is characterized by comprising the following steps: the rotation speed of ball milling in the step (1) is 350r/min, and the ball milling time is 12 h.
5. The molten salt method for preparing high-entropy rare earth tantalate (RETaO) according to claim 1 4 The method for preparing spherical powder is characterized by comprising the following steps: in the step (2), the drying is carried out at 90 ℃ for 24 hours, and the sieving is carried out by a 400-mesh sieve.
6. The molten salt method of claim 5 for preparing high-entropy rare earth tantalate (RETaO) 4 The method for preparing spherical powder is characterized by comprising the following steps: the calcining temperature in the step (2) is 800 ℃, and the time is 6 h.
7. The molten salt method for preparing high-entropy rare earth tantalate (RETaO) according to claim 1 4 The method for preparing spherical powder is characterized by comprising the following steps: and (4) drying at 90 ℃ for 24h, wherein the sieving is to sieve through 100 meshes and then through 400 meshes.
8. High entropy rare earth tantalate RETaO prepared by the process of any one of claims 1 to 7 4 Spherical powder.
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