CN112979311A - Nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering and method thereof - Google Patents
Nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering and method thereof Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 60
- 238000005245 sintering Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims description 26
- 239000000843 powder Substances 0.000 claims abstract description 42
- 238000000227 grinding Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 6
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims abstract description 4
- OSYUGTCJVMTNTO-UHFFFAOYSA-D oxalate;tantalum(5+) Chemical compound [Ta+5].[Ta+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O OSYUGTCJVMTNTO-UHFFFAOYSA-D 0.000 claims abstract description 3
- 238000004321 preservation Methods 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000000758 substrate Substances 0.000 claims description 3
- 238000002490 spark plasma sintering Methods 0.000 claims description 2
- 238000009766 low-temperature sintering Methods 0.000 claims 7
- 239000000463 material Substances 0.000 abstract description 18
- 238000002360 preparation method Methods 0.000 abstract description 12
- 239000012720 thermal barrier coating Substances 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 9
- 230000004888 barrier function Effects 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 11
- 239000002994 raw material Substances 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005262 decarbonization Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 238000007750 plasma spraying Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 230000000930 thermomechanical effect Effects 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052574 oxide ceramic Inorganic materials 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000357 thermal conductivity detection Methods 0.000 description 1
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Abstract
The invention belongs to the technical field of thermal barrier coating materials, and discloses a nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering and a preparation method thereof, wherein the structural formula of the ceramic is A4B2O9Wherein A is one or more of Ni, Co, Mg, Ca, Sr, Ba or Zn, and B is Ta; the preparation method of the ceramic comprises the following steps of A (OH)2、ACO3And the tantalum oxalate is respectively subjected to thermal decomposition for 1-2h at the temperature of 350-2O5Powder; then adding AO and Ta2O5Grinding the powder to obtain a nano-scale highly reactive powder mixture; and finally, performing discharge plasma sintering on the highly reactive powder mixture to prepare blocky A4B2O9 type tantalate ceramic. The invention solves the problems in the prior artThe cost of the thermal barrier coating and the environmental barrier coating material is high.
Description
Technical Field
The invention belongs to the technical field of thermal barrier coating materials, and particularly relates to nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering and a method thereof.
Background
In recent years, the rapid development of thermal barrier coatings and environmental barrier coating materials has led to the development and application of oxide ceramics of different types of crystal structures. Wherein the rare earth tantalate (RETaO)4、RE3TaO7And Reta3O9) Due to excellent thermo-mechanical properties (low thermal conductivity, high coefficient of thermal expansion, high fracture toughness, low modulus, high temperature stability, corrosion resistance, etc.), they are continuously studied and applied. However, the main raw material of the rare earth tantalate is rare earth elements, and the rare earth elements are protected as strategic resources in China, so that the exploitation amount of the rare earth elements is small, and the price of the rare earth elements is very high, so that the manufacturing cost of the rare earth tantalate is high.
In order to reduce the cost of thermal barrier coatings and materials for environmental barrier coatings, the inventors have studied the materials of thermal barrier coatings and materials for environmental barrier coatings to form tantalate ceramics of type A4B2O 9.
Disclosure of Invention
The invention aims to provide nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering and a method thereof, so as to solve the problem that the existing thermal barrier coating and environmental barrier coating materials are high in manufacturing cost.
In order to realize the purpose, the invention provides the following technical scheme that the nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering has a structural formula A4B2O9Wherein A is one or more of Ni, Co, Mg, Ca, Sr, Ba or Zn, and B is Ta.
The A4B2O9 type tantalate ceramic provided by the technical scheme has the characteristics of high compactness, high purity and nanocrystalline, and the hardness, fracture toughness and modulus of the ceramic material are very high, so that the thermophysical properties of the ceramic material can be regulated and controlled, and the A4B2O9 type tantalate ceramic can be used as a thermal barrier coating and an environmental barrier coating; moreover, the A4B2O9 type tantalate ceramics do not contain rare earth elements, so the manufacturing cost is relatively low.
The invention also provides another basic scheme, and the method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultralow temperature sintering comprises the following steps:
in the first step of the method,
a (OH)2、ACO3And the tantalum oxalate is respectively subjected to thermal decomposition at the temperature of 350-900 ℃ for 1-2h to obtain AO and Ta with high reaction activity2O5Powder;
in the second step, the first step is that,
reacting AO with Ta2O5Grinding the powder to obtain a nano-scale highly reactive powder mixture;
step three, performing a first step of cleaning the substrate,
and (3) performing spark plasma sintering on the highly reactive powder mixture to prepare blocky A4B2O9 type tantalate ceramic.
The beneficial effects of the technical scheme are as follows:
1. the blocky A4B2O9 type tantalate ceramic prepared by the technical scheme has the purity of more than 99 percent, the compactness of more than 98 percent and the average grain size of less than 300nm, and because the A4B2O9 type tantalate ceramic has fine and uniform nano crystals, phonons can be effectively scattered, the thermal conductivity of the material is reduced, and the heat insulation protection capability of the material is improved; the hardness, the fracture toughness and the modulus of the A4B2O9 type tantalate ceramic prepared by the method can be improved by high compactness, high purity and nanocrystalline, so that the A4B2O9 type tantalate ceramic has better thermophysical properties;
2. according to the technical scheme, the raw materials are subjected to thermal decomposition to form powder with high reactivity, so that the temperature required by the reaction between oxides during sintering can be reduced, the time can be shortened, the energy can be saved, and the efficiency can be improved; in addition, the problems of overburning and excessive growth of crystal grains generated by a common sintering method can be avoided, and the problems of high porosity and poor material thermo-mechanical property in the generated ceramic block are further avoided.
Further, in the second step, alcohol with the concentration of 99.99% is added during grinding, and the mass ratio of the powder to the alcohol is 1: 6-10.
Has the advantages that: can keep the powder moist, conveniently grind.
Further, in the second step, the rotation speed of the polishing is 2200-3000rpm, and the polishing time is 12-20 h.
Has the advantages that: by controlling the rotating speed and the grinding time, the nano-scale powder meeting the requirement can be obtained.
Further, in the second step, after grinding, taking out the powder, and preserving heat for 6-10h at 65-80 ℃.
Has the advantages that: and (3) carrying out heat preservation treatment on the powder after grinding to realize volatilization of alcohol mixed in the powder, and drying the powder.
Further, in the third step, the sintering temperature is 620-700 ℃, the heat preservation time is 6-10min, and the heat preservation pressure is 100-300 MPa.
Has the advantages that: sintering the powder into blocky A4B2O9 type tantalate ceramics can be realized by controlling the sintering temperature, the heat preservation time and the heat preservation pressure; meanwhile, the sintering temperature is low, the phenomena of overburning and excessive growth of crystal grains can be prevented, the formation and the maintenance of nano crystals are facilitated, and the energy consumption is low; and the time cost is also lower.
And further, in the third step, before sintering, spraying BN on the die.
Has the advantages that: and BN is sprayed before sintering, so that carbon in a sintering die can be prevented from permeating into the powder, and the high purity of the prepared blocky A4B2O9 type tantalate ceramic can be ensured. Meanwhile, the annealing and decarbonization process after sintering is avoided, and pores and cracks are introduced into the block body during annealing and decarbonization, so that the density of the material is reduced, and the technical scheme can ensure that the prepared blocky A4B2O9 type tantalate ceramic has high density.
Further, sintering the high-reactivity powder mixture obtained in the step two at 700 ℃ for 1-5h, cooling, and preparing the A in a spray granulation mode4B2O9And (3) forming tantalate spherical powder.
Has the advantages that: because the powder has high reactivity, the energy required by sintering is lower, the sintering can be completed at lower temperature, and the energy consumption is reduced; at the same time, the agglomeration phenomenon among the powder can be inhibited, so that the prepared A4B2O9The type tantalate spherical powder can be used as an atmospheric plasma spraying raw material for preparing a coating without grinding and sieving.
Description of the figures/tables
FIG. 1 is a comparison of the XRD diffractogram of example 1 of the present invention with a standard card;
FIG. 2 shows Ca provided in example 1 of the present invention4Ta2O9A surface micro-topography of the bulk ceramic;
FIG. 3 shows Ca provided in example 8 of the present invention2Mg2Ta2O9Schematic of thermal conductivity as a function of temperature.
Detailed Description
The following is further detailed by way of specific embodiments:
a nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering has a structural formula of A4B2O9Wherein A is one or more of Ni, Co, Mg, Ca, Sr, Ba or Zn, and B is Ta. The purity of the ceramic is more than 99%, the density is more than 98%, and the average grain size is less than 300 nm.
Example 1:
a nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering has a structural formula of Ca4Ta2O9The preparation method comprises the following steps:
in the first step of the method,
reacting Ca (OH)2、CaCO3Respectively preserving the oxalic acid at the temperature of 350-900 ℃ for 1-2h, and thermally decomposing the raw materials in the heat preservation process to obtain CaO and Ta with high reaction activity2O5And (3) powder. In the embodiment, the heat preservation temperature is preferably 900 ℃, and the heat preservation time is preferably 1 h.
In the second step, the first step is that,
according to Ca4Ta2O9The structural formula of (A) is to weigh CaO and Ta with high reactivity2O5Powdering and mixing highly reactive CaO and Ta2O5Putting the powder into a high-energy ball mill, putting 99.99% alcohol into the high-energy ball mill at a weight ratio of 1:6-10, and adding CaO and Ta at a rotation speed of 2200-2O5Grinding the powder for 12-20h, taking out the powder, and preserving heat at 65-80 ℃ for 6-10h to obtain a nanoscale high-reactivity powder mixture. In the embodiment, the weight ratio of the powder to the alcohol is 1:8, the rotation speed during grinding is preferably 2200rpm, and the grinding time is preferably 16 h; after grinding, the temperature for heat preservation is preferably 75 ℃, and the time for heat preservation is preferably 6 hours.
Step three, performing a first step of cleaning the substrate,
spraying BN treatment on the graphite mold for sintering, and putting the nano-scale highly reactive powder mixture formed in the step two into the graphite mold for sintering at the sintering temperature of 620-300 MPa, the heat preservation time of 6-10min and the heat preservation pressure of 100-300MPa to obtain the blocky Ca-containing material4Ta2O9A ceramic. In this embodiment, the sintering temperature is preferably 620 ℃, the heat preservation time is preferably 10min, and the heat preservation pressure is preferably 150 MPa.
Example 2:
example 2 is different from example 1 in that the structure of the A4B2O9 type tantalate ceramic in this example is Ni4Ta2O9The preparation process is identical to example 1.
Example 3:
example 3 is different from example 1 in that the structure of the A4B2O9 type tantalate ceramic in this example is Co4Ta2O9The preparation process is identical to example 1.
Example 4:
example 4 is different from example 1 in that the A4B2O9 type tantalate ceramic in this example has the structural formula of Mg4Ta2O9The preparation process is identical to example 1.
Example 5:
example 5 differs from example 1 in that the A4B2O9 type tantalate ceramic in this example has the structural formula Sr4Ta2O9The preparation process is identical to example 1.
Example 6:
example 6 is different from example 1 in that the structural formula of the A4B2O9 type tantalate ceramic in this example is Ba4Ta2O9The preparation process is identical to example 1.
Example 7:
example 7 is different from example 1 in that the A4B2O9 type tantalate ceramic in this example has a structural formula of Zn4Ta2O9The preparation process is identical to example 1.
Example 8:
example 8 is different from example 1 in that the structure of the A4B2O9 type tantalate ceramic in this example is Ca2Mg2Ta2O9(ii) a The preparation method is different from the embodiment 1 in that the heat preservation temperature of the thermal decomposition in the step one is 545 ℃ and the heat preservation time is 2 hours; in the second step, the rotation speed during grinding is 2800rpm, the grinding time is 20h, the heat preservation temperature after grinding is 80 ℃, and the heat preservation time is 8 h; the sintering temperature in the third step is 650 ℃, the heat preservation time is 8min, and the heat preservation pressure is 200 Mpa.
Example 9:
example 9 differs from example 8 in that the structure of the A4B2O9 type tantalate ceramic in this example is CaMgZnBaTa2O9(ii) a The preparation method is different from the embodiment 1 in that the heat preservation temperature of the thermal decomposition in the step one is 350 ℃, and the heat preservation time is 1 h; in the second step, the rotation speed during grinding is 3000rpm, the grinding time is 12 hours, the heat preservation temperature after grinding is 65 ℃, and the heat preservation time is 10 hours; in the third step, the sintering temperature is 680 ℃, the heat preservation time is 6min, and the heat preservation pressure is 230 Mpa.
Example 10:
example 10 differs from example 9 in that in this example, the third step is a stepPutting the nano-scale highly reactive powder mixture into a high-temperature sintering furnace, sintering at 700 ℃ for 1-5h, taking out the sintered powder, cooling, and preparing the CaMgZnBaTa by using a spray granulation method2O9The ceramic powder prepared is spherical, can be used as an air plasma spraying raw material for preparing a coating, and the sintering time is preferably 1h in the embodiment. The purity of the powder can be obtained by XRD test, and the result is consistent with that of figure 1.
Experiment:
the nanocrystalline A4B2O9 type tantalate ceramics provided in examples 1-9 were selected for the following experiments:
characterization by XRD
The tantalate ceramic blocks type A4B2O9 obtained in examples 1 to 9 were examined using an X-ray diffractometer, wherein the XRD pattern of example 1 is shown in fig. 1. According to the results shown in FIG. 1, Ca4Ta2O9The diffraction peaks of the ceramics correspond to the standard PDF #31-0308 one by one.
SEM characterization
The A4B2O9 type tantalate ceramic blocks prepared in examples 1-9 were examined by scanning electron microscopy, wherein the surface micro-topography of example 1 is shown in FIG. 2. As can be seen from FIG. 2, Ca4Ta2O9The grain size of the ceramic is uniform, the grain size is less than 300nm, the grain boundary is clear, no obvious air holes and cracks exist on the surface, and the density is as high as 99.5%.
3. Thermal conductivity detection
The ceramic blocks obtained in examples 1 to 9 were polished into round sheets having a diameter of 6X 1mm, and the thermal conductivity thereof was measured by a laser thermal conductivity meter, wherein the thermal conductivity of each of the ceramic blocks of examples 1 to 9 at 900 ℃ is shown in Table 1, and the Ca provided in example 8 at room temperature to 900 ℃ is measured2Mg2Ta2O9The thermal conductivity curve of the ceramic block is shown in fig. 3. As can be seen from fig. 3, the thermal conductivity of the ceramic block decreases sharply with increasing temperature, and decreases slowly after 600 ℃. At a temperature of 900 ℃ Ca2Mg2Ta2O9Thermal conductivity of ceramic blocksReduced to 1.4W.m-1.K-1Thus, the material has excellent heat insulation capability in high-temperature environment.
4. Density detection
The ceramic blocks provided in examples 1-9 were tested using archimedes' drainage.
The results of the experiments on the tantalate ceramics type A4B2O9 provided in examples 1 to 9 are shown in table 1.
TABLE 1
| Structural formula (I) | Young's modulus | Hardness of | Thermal conductivity | Compactness degree | |
| Example 1 | Ca4Ta2O9 | 186 | 9.2 | 2.1-5.2 | 99.5 |
| Example 2 | Ni4Ta2O9 | 163 | 7.6 | 1.5-4.3 | 99.0 |
| Example 3 | Co4Ta2O9 | 201 | 10.9 | 2.3-6.0 | 99.7 |
| Example 4 | Mg4Ta2O9 | 144 | 7.1 | 1.2-3.9 | 99.6 |
| Example 5 | Sr4Ta2O9 | 169 | 8.0 | 1.8-4.6 | 99.0 |
| Example 6 | Ba4Ta2O9 | 210 | 12.5 | 2.5-3.9 | 99.1 |
| Example 7 | Zn4Ta2O9 | 152 | 6.6 | 2.0-4.3 | 99.3 |
| Example 8 | Ca2Mg2Ta2O9 | 162 | 8.3 | 1.4-4.2 | 99.8 |
| Example 9 | CaMgZnBaTa2O9 | 180 | 10.6 | 1.3-3.7 | 99.1 |
In conclusion, the A4B2O9 type tantalate ceramic provided by the invention has the purity of more than 99%, the compactness of more than 98%, the average grain size of less than 300nm, and low thermal conductivity at high temperature, and can be used as a thermal barrier coating material and an environmental barrier coating material. Compared with the existing rare earth tantalate thermal barrier coating material, the rare earth tantalate thermal barrier coating material does not use rare earth elements in raw materials, has low preparation cost and is more suitable for use and research.
It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention, and these changes and modifications should not be construed as affecting the performance of the invention and its practical application.
Claims (8)
1. A nanocrystalline A4B2O9 type tantalate ceramic prepared by ultralow temperature sintering is characterized in that: the structural formula of the ceramic is A4B2O9Wherein A is one or more of Ni, Co, Mg, Ca, Sr, Ba or Zn, and B is Ta.
2. The method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultra-low temperature sintering according to claim 1, comprising the following steps:
in the first step of the method,
a (OH)2、ACO3And the tantalum oxalate is respectively subjected to thermal decomposition at the temperature of 350-900 ℃ for 1-2h to obtain AO and Ta with high reaction activity2O5Powder;
in the second step, the first step is that,
reacting AO with Ta2O5Grinding the powder to obtain a nano-scale highly reactive powder mixture;
step three, performing a first step of cleaning the substrate,
and (3) performing spark plasma sintering on the highly reactive powder mixture to prepare blocky A4B2O9 type tantalate ceramic.
3. The method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultra-low temperature sintering according to claim 2, wherein the method comprises the following steps: in the second step, alcohol with the concentration of 99.99% is added during grinding, and the mass ratio of the powder to the alcohol is 1: 6-10.
4. The method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultra-low temperature sintering according to claim 2, wherein the method comprises the following steps: in the second step, the rotation speed of the polishing is 2200-3000rpm, and the polishing time is 12-20 h.
5. The method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultra-low temperature sintering according to claim 2, wherein the method comprises the following steps: in the second step, after grinding, the powder is taken out and kept at 65-80 ℃ for 6-10 h.
6. The method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultra-low temperature sintering according to claim 2, wherein the method comprises the following steps: in the third step, the sintering temperature is 620-700 ℃, the heat preservation time is 6-10min, and the heat preservation pressure is 100-300 MPa.
7. The method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultra-low temperature sintering according to claim 2, wherein the method comprises the following steps: and in the third step, spraying BN on the die before sintering.
8. The method for preparing the nanocrystalline A4B2O9 type tantalate ceramic by ultra-low temperature sintering according to claim 2, wherein the method comprises the following steps: sintering the highly reactive powder mixture obtained in the step two at 700 ℃ for 1-5h, cooling, and preparing A in a spray granulation mode4B2O9And (3) forming tantalate spherical powder.
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