CN109928763B - Tantalum-based oxynitride nano powder and preparation method thereof - Google Patents
Tantalum-based oxynitride nano powder and preparation method thereof Download PDFInfo
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 36
- 229910052715 tantalum Inorganic materials 0.000 title claims abstract description 34
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001354 calcination Methods 0.000 claims abstract description 35
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000000498 ball milling Methods 0.000 claims abstract description 12
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 10
- -1 alkaline earth metal salt Chemical class 0.000 claims abstract description 10
- 150000003481 tantalum Chemical class 0.000 claims abstract description 10
- 239000012298 atmosphere Substances 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 229910002355 SrTaO2N Inorganic materials 0.000 claims description 7
- 229910002937 BaTaO2N Inorganic materials 0.000 claims description 6
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 claims description 6
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 claims description 6
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 4
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical group O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims description 4
- 229910000018 strontium carbonate Inorganic materials 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
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- 125000004429 atom Chemical group 0.000 description 3
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- 229920000877 Melamine resin Polymers 0.000 description 1
- 229910003071 TaON Inorganic materials 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
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- 239000003990 capacitor Substances 0.000 description 1
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 150000004767 nitrides Chemical class 0.000 description 1
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- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 238000005580 one pot reaction Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明公开了一种钽基氧氮化物纳米粉的制备方法，包括以下步骤：S1、将碱土金属盐、钽盐与氮源溶于醇中，球磨后干燥，得到混合前驱体；S2、将步骤S1所得的混合前驱体置于反应容器内，在保护气氛下进行无压放电等离子煅烧，得到钽基氧氮化物纳米粉，本发明的制备方法制备周期短，制备得到的钽基氧氮化物纳米粉纯度高。
The invention discloses a preparation method of tantalum-based oxynitride nano-powder, comprising the following steps: S1, dissolving an alkaline earth metal salt, a tantalum salt and a nitrogen source in alcohol, ball-milling and drying to obtain a mixed precursor; S2, dissolving an alkaline earth metal salt, a tantalum salt and a nitrogen source in an alcohol The mixed precursor obtained in step S1 is placed in a reaction vessel, and subjected to pressureless discharge plasma calcination in a protective atmosphere to obtain tantalum-based oxynitride nano-powder. The preparation method of the present invention has a short preparation period, and the prepared tantalum-based oxynitride Nano powder is of high purity.
Description
Technical Field
The invention relates to the technical field of preparation of high-performance dielectric ceramic materials, in particular to tantalum-based oxynitride nano powder and a preparation method thereof.
Background
Perovskite oxynitride SrTaO2N and BaTaO2N has a very high dielectric constant at room temperature, and thus has attracted extensive attention of domestic and foreign scholars. In the two crystal structures, Ta atom and O/N atom form Ta (O, N)6Octahedron with Ta in the center of the octahedron, A atoms between the octahedron and occupying the eight vertices of the unit cell, Ta (O, N) due to the difference in radii of A and Ta atoms and the multiple arrangement of N atoms6The octahedron is inclined to different degrees, the bond length and bond angle of Ta-O/N-Ta are changed, and Ta ions deviate from the central position to generate spontaneous polarization. Besides excellent dielectric properties, the materials also have the advantages of metal oxides and nitrides, have good thermal stability and acid-base corrosion resistance, and are considered to be ideal materials for novel high-performance capacitors.
At present, SrTaO2N and BaTaO2The synthesis method of the N nano powder mainly comprises a two-step method and a one-step method. Two-step method, namely synthesizing composite oxide precursor (Sr) containing multiple metal cations2Ta2O7And Ba5Ta4O15) And then in a flowing ammonia atmosphere at an elevated temperature (>1000 ℃) were aminated. Since the gas-solid reaction is slowly diffused during the ammoniation process, the nano powder is repeatedly stopped and ground in the middle of the reaction to improve the yield, and the preparation time of only the calcination step is usually as long as tens of hours. One-step method, i.e. without using ammonia gas or directly using ammonia gas, adopts Ta3N5TaON, urea,Melamine and the like as a nitrogen source, and oxynitride is synthesized by a one-step reaction. This method greatly improves the reaction efficiency, but the preparation time still takes several hours. Meanwhile, when the temperature rise rate is too slow in the conventional calcination, the nitrogen source such as urea is completely decomposed at a temperature lower than the temperature at which the oxynitride is generated, and the nitrogen source is largely lost, so that the nitriding efficiency is low, and the purity of the oxynitride in the product is also lowered.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects of the prior art and provide high-purity tantalum base oxynitride nano powder, and correspondingly, the invention also provides a preparation method of the tantalum base oxynitride nano powder, which has the advantages of short preparation period, low cost and high purity.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of tantalum-based oxynitride nano powder comprises the following steps:
s1, dissolving alkaline earth metal salt, tantalum salt and a nitrogen source in alcohol, and drying after ball milling to obtain a mixed precursor;
s2, placing the mixed precursor obtained in the step S1 in a reaction container, and performing discharge plasma calcination in a protective atmosphere to obtain the tantalum-based oxynitride nano powder.
As a further improvement to the above technical solution:
preferably, in step S2, the calcination includes: heating to 800-1400 ℃ at a heating rate of 50-500 ℃/min, preserving the heat for 1-30 min, and cooling to room temperature along with the furnace.
More preferably, in step S2, the calcination specifically comprises: heating to 900-1300 ℃ at the heating rate of 50-300 ℃/min, preserving the heat for 1-10 min, and cooling to room temperature along with the furnace.
Preferably, in step S2, the reaction vessel includes a vessel shell, the top and the bottom of the vessel shell are symmetrically provided with circular truncated cone covers, and the side wall of the vessel shell is provided with more than two through holes.
Preferably, the bottom surface of the circular table cover is arranged close to one side of the container shell.
Preferably, the through holes are symmetrically arranged near one side of the top of the container shell.
Preferably, in step S1, the alkaline earth metal salt is strontium carbonate or barium carbonate, the tantalum salt is tantalum pentoxide, the nitrogen source is urea, and the alcohol is absolute ethanol.
Preferably, the mass volume ratio of the alkaline earth metal salt, the tantalum salt, the nitrogen source and the alcohol is 1-8 g: 2-8 g: 0.1-10 g: 5-100 mL.
More preferably, the ratio of the alkaline earth metal salt, tantalum salt, nitrogen source and alcohol is 2g to 6 g: 0.5g to 6 g: 5mL to 50 mL.
Preferably, in step S1, the drying specifically includes: keeping the temperature for 1 to 72 hours at the temperature of between 30 and 80 ℃.
More preferably, the drying temperature is 50-80 ℃, and the drying time is 6-48 h.
Preferably, the protective atmosphere is one or more of nitrogen, helium or argon.
As a general inventive concept, the present invention also provides a tantalum based oxynitride nanopowder prepared by the foregoing preparation method.
Compared with the prior art, the invention has the advantages that:
1. the method adopts the combination of discharge plasma calcination and a nitrogen source one-step synthesis method to prepare the tantalum-based oxynitride, has high heat transfer efficiency and very high heating efficiency due to joule effect and electric field effect, only needs several minutes in the whole process, greatly shortens the preparation time compared with the traditional preparation method (several hours or even tens of hours), has lower cost, has rapid temperature rise of discharge plasma sintering, and can dynamically inhibit the decomposition of the nitrogen source.
2. The invention adopts a rapid heating-up mode with a heating-up rate of 50 ℃/min-300 ℃/min, compared with the traditional calcining mode (the heating-up rate is 1 ℃/min-50 ℃/min), the invention can further inhibit the decomposition of a nitrogen source from the aspect of chemical kinetics, and the temperature of a reaction system can rapidly reach the temperature required by the generation of oxynitride on the premise of keeping a large amount of nitrogen source, thereby generating sufficient nitridation reaction, greatly shortening the reaction time and improving the purity of the product.
3. The reaction vessel for placing the raw material mixed nano powder comprises a vessel shell, wherein the top and the bottom of the vessel shell are symmetrically provided with the circular table covers, the circular table covers are small in cross section area relative to the traditional cylindrical cover, the corresponding current density is large, more joule heat is generated, and the reaction vessel is higher in heat transfer efficiency and better in effect relative to the traditional cylindrical cover, is beneficial to energy conservation and cost reduction, and reduces the reaction temperature to a certain extent.
Drawings
FIG. 1 is a schematic diagram of a reaction vessel and a sample in example 1 of the present invention.
FIG. 2 is an XRD spectrum of the TaNxNy powder prepared in example 1 of the present invention.
FIG. 3 is an SEM photograph of the TaNbOx nano-powder obtained in example 1 of the present invention.
FIG. 4 is an XRD spectrum of the TaNbOx nano powder prepared in example 2 of the present invention.
FIG. 5 is an SEM photograph of the TaNbOx nano-powder obtained in example 2 of the present invention.
The reference numerals in the figures denote:
1. a container housing; 11. a through hole; 12. a circular table cover; 2. and mixing the precursors.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The starting materials and equipment used in the following examples are commercially available.
The invention relates to a rapid preparation method of tantalum-based oxynitride nano powder, which comprises the following steps:
s1, dissolving alkaline earth metal salt, tantalum salt and a nitrogen source in alcohol, and drying after ball milling to obtain a mixed precursor;
s2, placing the mixed precursor obtained in the step S1 in a reaction container, and performing discharge plasma calcination in a protective atmosphere to obtain the tantalum-based oxynitride nano powder.
The method adopts the mode of combining discharge plasma calcination with a nitrogen source one-step synthesis method to prepare the tantalum-based oxynitride, has very high heating efficiency due to joule effect and electric field effect, only needs several minutes in the whole process, greatly shortens the preparation time compared with the traditional preparation method (several hours to tens of hours), and has lower cost.
Example 1:
the rapid preparation method of tantalum-based oxynitride nano powder of the embodiment comprises the following steps:
s1, adding 3.5g of strontium carbonate, 4.5g of tantalum pentoxide and 4.8g of urea into 35ml of absolute ethyl alcohol, and carrying out ball milling for 240min to obtain mixed slurry;
s2, drying the mixed slurry obtained after ball milling in the step S1, wherein the drying process comprises the following steps: preserving the heat for 24 hours at the temperature of 60 ℃ to obtain a mixed precursor;
s3, placing the mixed precursor obtained in the step S2 in a reaction container, placing the reaction container in a non-pressure plasma calcining device, and performing discharge plasma calcining in a nitrogen atmosphere, wherein the heating rate is 300 ℃/min, the temperature is 1000 ℃, and the heat preservation time is 1 min; finally cooling to room temperature along with the furnace to obtain SrTaO2The phase composition and the micro-morphology of the N-oxynitride powder, i.e., the tantalum-based oxynitride nanopowder, are shown in fig. 2 and 3, respectively.
In the present invention, "pressureless" in pressureless plasma calcination means no mechanical pressure, not vacuum. In the conventional spark plasma sintering, the powdered mixed precursor is densified under the condition of mechanical pressure application, and finally a bulk material is obtained. The discharge plasma calcination of the invention is to calcine the mixed powder precursor under the condition of no mechanical pressure, and finally obtain the powder material.
As shown in fig. 1, the reaction vessel includes a vessel shell 1 which is a hollow cylindrical graphite crucible, the top and the bottom of the vessel shell 1 are symmetrically provided with a circular table cover 12, the side wall of the vessel shell 1 is provided with more than two through holes 11, the mixture precursor 2 is laid in the vessel shell 1, and 2 through holes 11 are symmetrically arranged near one side of the top of the vessel shell 1; the circular table cover 12 is a graphite cover, and the bottom surface of the circular table cover 12 is arranged close to one side of the container shell 1.
As can be seen from FIGS. 2 and 3, SrTaO prepared in this example2The N-oxynitride powder is almost pure phase SrTaO2N, the color is bright yellow green; the shape and size of the crystal grains are uniform, and the size of the crystal grains is about 50-150 nm.
Comparative example 1:
the preparation method of the tantalum base oxynitride nano powder of the comparative example is almost the same as that of the embodiment 1, and the difference is that:
in step S3, the non-pressure plasma sintering equipment is not used for the spark plasma calcination, the conventional non-pressure sintering furnace is used for the ordinary calcination, the reaction vessel is a crucible (sealed vessel) with a cover, the temperature rise rate of the calcination is 20 ℃/min, the calcination temperature is 1100 ℃, and the heat preservation time is 60 min.
SrTaO prepared in this comparative example2The N oxynitride powder phase composition is SrTaO2N (small amount), Sr2Ta2O7(a large amount) and Ta3N5(small amount), the color is off-white, and the purity is lower than that of the example 1 through qualitative analysis by comparing with the color of the tantalum oxynitride nano powder in the example 1. Therefore, by adopting the discharge plasma calcination, the oxynitride powder with higher purity can be obtained only by lower temperature and shorter heat preservation time than the conventional method.
Example 2:
the rapid preparation method of tantalum-based oxynitride nano powder of the embodiment comprises the following steps:
s1, adding 4.8g of barium carbonate, 4.5g of tantalum pentoxide and 4.8g of urea into 40ml of absolute ethyl alcohol, and carrying out ball milling for 240min to obtain mixed slurry;
s2, drying the mixed slurry obtained after ball milling in the step S1, wherein the drying process comprises the following steps: preserving the heat for 24 hours at the temperature of 60 ℃ to obtain a mixed precursor;
s3, placing the mixed precursor obtained in the step S2 into a reaction container, placing the reaction container into a non-pressure plasma calcining device, and performing discharge plasma calcining in a nitrogen atmosphere, wherein the temperature rise rate is 300 ℃/min, the temperature is 1000 ℃, and the temperature is keptThe time is 1 min; finally, cooling to room temperature along with the furnace to obtain BaTaO2The phase composition and the micro-morphology of the N-oxynitride powder, i.e., the tantalum-based oxynitride nanopowder, are shown in fig. 4 and 5, respectively.
The reaction vessel used in this example was the same as in example 1.
As is clear from FIGS. 4 and 5, BaTaO produced in this example2The N-oxynitride powder is almost pure phase BaTaO2N, the color is brown; the shape and size of the crystal grains are uniform, and the size of the crystal grains is about 50-150 nm.
Comparative example 2:
the preparation method of the tantalum base oxynitride nano powder of the comparative example is almost the same as that of the embodiment 1, and the difference is that:
in step S3, the non-pressure plasma calcination device is not used for discharge plasma calcination, the conventional non-pressure calciner is used for ordinary calcination, the reaction vessel is a crucible (sealed vessel) with a cover, the temperature rise rate of calcination is 20 ℃/min, the calcination temperature is 1100 ℃, and the heat preservation time is 60 min.
BaTaO prepared in this comparative example2The N oxynitride powder phase composition is BaTaO2N (small amount), Ba5Ta4O15(a large amount) and Ta3N5(small amount), the color is off-white, and the purity is lower than that of the example 2 through qualitative analysis by comparing with the color of the tantalum oxynitride nano powder in the example 2. Therefore, by adopting the discharge plasma calcination, the oxynitride powder with higher purity can be obtained only by lower temperature and shorter heat preservation time than the conventional method.
Example 3:
the rapid preparation method of tantalum-based oxynitride nano powder of the embodiment comprises the following steps:
s1, adding 3.5g of strontium carbonate, 4.5g of tantalum pentoxide and 4.8g of urea into 40ml of absolute ethyl alcohol, and carrying out ball milling for 240min to obtain mixed slurry;
s2, drying the mixed slurry obtained after ball milling in the step S1, wherein the drying process comprises the following steps: preserving the heat for 24 hours at the temperature of 60 ℃ to obtain a mixed precursor;
s3, placing the mixed precursor obtained in the step S2 in a reaction container, placing the reaction container in non-pressure plasma calcination equipment, and performing discharge plasma calcination in a nitrogen atmosphere, wherein the heating rate is 200 ℃/min, the temperature is 1100 ℃, and the heat preservation time is 1 min; finally cooling to room temperature along with the furnace to obtain SrTaO2N oxynitride powder, i.e., tantalum oxynitride nanopowder.
The reaction vessel used in this example was the same as in example 1.
Through detection, the SrTaO prepared in the embodiment2The N-oxynitride powder is almost pure phase SrTaO2N, the color is bright yellow green; the shape and size of the crystal grains are uniform, and the size of the crystal grains is about 100-200 nm.
Example 4:
the rapid preparation method of tantalum-based oxynitride nano powder of the embodiment comprises the following steps:
s1, adding 4.8g of barium carbonate, 4.5g of tantalum pentoxide and 4.8g of urea into 40ml of absolute ethyl alcohol, and carrying out ball milling for 240min to obtain mixed slurry;
s2, drying the mixed slurry obtained after ball milling in the step S1, wherein the drying process comprises the following steps: preserving the heat for 24 hours at the temperature of 60 ℃ to obtain a mixed precursor;
s3, placing the mixed precursor obtained in the step S2 in a reaction container, placing the reaction container in non-pressure plasma calcination equipment, and performing discharge plasma calcination in a nitrogen atmosphere, wherein the heating rate is 200 ℃/min, the temperature is 1100 ℃, and the heat preservation time is 1 min; finally, cooling to room temperature along with the furnace to obtain BaTaO2N oxynitride powder, i.e., tantalum oxynitride nanopowder.
The reaction vessel used in this example was the same as in example 1.
Through detection, the BaTaO prepared in the example2The N-oxynitride powder is almost pure phase BaTaO2N, the color is brown; the shape and size of the crystal grains are uniform, and the size of the crystal grains is about 100-200 nm.
Comparative example 3:
the preparation method of the tantalum base oxynitride nanopowder of the comparative example is substantially the same as that of example 1, except that in step S3, the upper and lower covers of the reaction vessel are conventional cylindrical covers, the height of the cylindrical covers is the same as that of the truncated cone cover in example 1, and the cross section of the cylindrical covers is the same as that of the bottom surface of the truncated cone cover.
In the calcining process, the output power required by the equipment is higher than that of the embodiment 1, namely, the energy consumption of the cylindrical cover with the same technological parameters is high, the heat transfer efficiency is low, the reaction vessel adopting the invention is more energy-saving, is beneficial to reducing the cost and reduces the reaction temperature to a certain extent.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments to equivalent variations, without departing from the scope of the invention, using the teachings disclosed above. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (8)
1. A preparation method of tantalum-based oxynitride nano powder is characterized by comprising the following steps: the method comprises the following steps:
s1, dissolving alkaline earth metal salt, tantalum salt and a nitrogen source in alcohol, and drying after ball milling to obtain a mixed precursor; the alkaline earth metal salt is strontium carbonate or barium carbonate, the tantalum salt is tantalum pentoxide, the nitrogen source is urea, the alcohol is absolute ethyl alcohol, and the mass-volume ratio of the alkaline earth metal salt to the tantalum salt to the nitrogen source to the alcohol is 1-8 g: 2-8 g: 0.1-10 g: 5-100 mL
S2, placing the mixed precursor obtained in the step S1 in a reaction container, and carrying out non-pressure discharge plasma calcination under a protective atmosphere to obtain tantalum base oxynitride nano powder; the tantalum-based oxynitride is perovskite oxynitride SrTaO2N or BaTaO2N; in the step S2, the calcination specifically includes: heating to 800-1400 ℃ at a heating rate of 50-500 ℃/min, preserving heat for 1-30 min, and cooling with the furnaceAnd (4) cooling to room temperature.
2. The method of claim 1, wherein: in the step S2, the calcination specifically includes: heating to 900-1300 ℃ at the heating rate of 50-300 ℃/min, preserving the heat for 1-10 min, and cooling to room temperature along with the furnace.
3. The production method according to claim 1 or 2, characterized in that: in the step S2, the reaction vessel includes a vessel shell (1), circular platform covers (12) are symmetrically disposed on the top and the bottom of the vessel shell (1), and more than two through holes (11) are disposed on the side wall of the vessel shell (1).
4. The production method according to claim 3, characterized in that: the bottom surface of the circular table cover (12) is arranged close to one side of the container shell (1).
5. The method of claim 4, wherein: the through holes (11) are close to one side of the top of the container shell (1) and are symmetrically arranged.
6. The production method according to claim 1 or 2, characterized in that: in step S1, the drying specifically includes: keeping the temperature for 1 to 72 hours at the temperature of between 30 and 80 ℃.
7. The production method according to claim 1 or 2, characterized in that: the protective atmosphere is one or more of nitrogen, helium or argon.
8. A tantalum-based oxynitride nano powder is characterized in that: the tantalum oxynitride nano powder is prepared by the preparation method of any one of claims 1 to 7.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910171688.2A CN109928763B (en) | 2019-03-07 | 2019-03-07 | Tantalum-based oxynitride nano powder and preparation method thereof |
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| CN201910171688.2A CN109928763B (en) | 2019-03-07 | 2019-03-07 | Tantalum-based oxynitride nano powder and preparation method thereof |
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| Publication Number | Publication Date |
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| CN109928763A CN109928763A (en) | 2019-06-25 |
| CN109928763B true CN109928763B (en) | 2022-03-29 |
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