CN113213926B - Ta 2 O 5 Ceramic target material and preparation method thereof - Google Patents
Ta 2 O 5 Ceramic target material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a Ta 2 O 5 The preparation method of the ceramic target comprises the following steps: step one, ta (OH) 5 The powder is sequentially calcined at low temperature and high temperature to obtain Ta 2 O 5 Powder; the low-temperature calcination temperature is 600-750 ℃, the low-temperature calcination time is 3-6 hours, and the low-temperature calcination atmosphere is air atmosphere; the high-temperature calcination temperature is 800-1200 ℃, the high-temperature calcination time is 2-8 hours, and the high-temperature calcination atmosphere is oxygen atmosphere; step two, adding deionized water and a dispersing agent into Ta 2 O 5 In the powder to obtain Ta 2 O 5 Grinding, atomizing, granulating, agglomerating, molding, cold isostatic pressing and sintering in normal-pressure oxygen atmosphere to obtain Ta for coating 2 O 5 A ceramic target material. The invention also provides a Ta 2 O 5 A ceramic target material. Ta of the invention 2 O 5 The ceramic target has small porosity and high density (the relative density is more than or equal to 99%).
Description
Technical Field
The invention belongs to the technical field of coating materials, and particularly relates to Ta 2 O 5 A ceramic target material and a preparation method thereof.
Background
Ta 2 O 5 As a coating material, the spectral transmission band of the film is 0.3-10 μm, and the film is one of important high-refractive-index materials in the visible light to near-infrared band. Ta 2 O 5 The film has high refractive index (2.1), thermal stability, low absorption, high mechanical strength, strong laser damage resistance, amorphous microstructure and chemical resistanceCorrosion and the like, and can be widely applied to the field of optical multilayer films such as high-reflection films, antireflection films, light splitting films, light filtering films and the like for preparing various optical elements. The film is prepared by using a target material as a coating material and using methods such as Radio Frequency (RF) magnetron sputtering, pulsed Laser Deposition (PLD), ion beam sputtering and the like. Preparation of film, ta, by the above-described method 2 O 5 The characteristics of the target material have important influence on the film performance, such as target density, chemical composition morphology and the like. Because a large number of micro-pores are arranged on the surface and inside of the low-density target material, the target material surface is easy to be pulverized and nodulated in the coating process, and the yield and the production efficiency of the film are reduced. At the same time, ta 2 O 5 The oxygen loss generated by high-temperature sintering under vacuum and reduction conditions can generate the coexistence of low-valence tantalum oxides such as tantalum trioxide and tantalum dioxide, and the film forming rates of the different-valence tantalum oxides are different, which is not beneficial to the stability and consistency of film production.
Disclosure of Invention
An object of the present invention is to provide a Ta 2 O 5 The method for preparing the ceramic target can prepare Ta with small porosity and high density (the relative density is more than or equal to 99 percent) 2 O 5 A ceramic target material.
The second object of the present invention is to provide a Ta 2 O 5 A ceramic target material.
In order to achieve one of the purposes, the invention adopts the following technical scheme:
ta 2 O 5 The preparation method of the ceramic target comprises the following steps:
step one, ta (OH) 5 The powder is sequentially calcined at low temperature and high temperature to obtain Ta 2 O 5 Powder;
the low-temperature calcination temperature is 600-750 ℃, the low-temperature calcination time is 3-6 hours, and the low-temperature calcination atmosphere is air atmosphere;
the high-temperature calcination temperature is 800-1200 ℃, the high-temperature calcination time is 2-8 hours, and the high-temperature calcination atmosphere is oxygen atmosphere;
step two, will getIonic water and dispersant adding Ta 2 O 5 In the powder, ta is obtained 2 O 5 Grinding, atomizing, granulating, agglomerating, molding, cold isostatic pressing and sintering in normal-pressure oxygen atmosphere to obtain Ta for coating 2 O 5 A ceramic target material.
The invention removes chemically bound water and surface adsorbed NOx and F through thermal decomposition of low-temperature calcination - The volatile impurities are equal to obtain orthorhombic Ta 2 O 5 (ii) a High-temperature calcination is carried out to realize recrystallization, obtain certain crystal form, crystal size, pore structure and specific surface, and improve Ta 2 O 5 The crystallinity of the powder ensures the uniformity of the particle size and improves the microstructure property of the powder; adopts the atmospheric oxygen atmosphere sintering to avoid Ta 2 O 5 Sintering the tantalum oxide with low valence state generated by oxygen loss at high temperature under vacuum and reduction conditions to obtain Ta with no oxygen loss, single property, small porosity and high density 2 O 5 A ceramic target material.
Further, in step one, the Ta (OH) 5 The purity of the powder is 4N, and the specific surface area is 50-100 m 2 /g；
Said Ta 2 O 5 The specific surface area of the powder is 5 to 25m 2 /g。
Further, in the second step, the deionized water, the dispersant and Ta 2 O 5 The mass ratio of the powder is 35-65, 0.1-1.0 and 100.
Further, the dispersing agent is one of octadecylamine ammonium acetate, cis-9-octadecenoic acid and polyethylene glycol 600.
Further, in step two, the ground Ta 2 O 5 The grain size of the slurry is less than or equal to 0.5 mu m;
the process conditions of atomization granulation are as follows: the centrifugal rotating speed is 12000-25000 rpm, and the hot air outlet temperature is 100-130 ℃;
agglomerated Ta 2 O 5 The particle size of the slurry is 50-120 mu m.
Further, in the second step, the pressure of the mould pressing is 300-600Kg/cm 2 。
Further, in the second step, the pressure of the cold isostatic pressing is 240-300 MPa, and the pressure maintaining time is 5-20 min.
Further, in the second step, the process conditions of the atmospheric pressure oxygen atmosphere sintering are as follows: the sintering temperature is 1200-1550 ℃, and the heat preservation time is 3-12 hours.
Further, in step two, said Ta 2 O 5 The relative density of the ceramic target material is more than or equal to 99 percent.
In order to achieve the second purpose, the invention adopts the following technical scheme:
ta 2 O 5 Ceramic target material, said Ta 2 O 5 The ceramic target is obtained by the preparation method.
Further, said Ta 2 O 5 The relative density of the ceramic target material is more than or equal to 99 percent.
The invention has the beneficial effects that:
the invention adopts secondary calcination to prepare Ta 2 O 5 The powder is sintered in the atmosphere of oxygen at normal pressure, so that the high density (the relative density is more than or equal to 99 percent), no oxygen loss and single-phase Ta meeting the stoichiometric ratio are easily realized 2 O 5 The ceramic industrialized production method has the advantages of high growth rate and keeping the consistency of the film and the target components by using the target material for coating.
Detailed Description
The following detailed description of specific embodiments of the invention.
Example 1:
1. the purity is 4N, the specific surface area is 80m 2 Ta (OH) per g 5 The powder is sequentially calcined at low temperature and high temperature to obtain 18m 2 Ta of specific surface area/g 2 O 5 And (3) powder. Wherein the low-temperature calcination temperature is 700 ℃, and the air atmosphere is kept for 5 hours. The high-temperature calcination temperature is 1000 ℃, the high-temperature calcination time is 5 hours, and the high-temperature calcination atmosphere is an oxygen atmosphere.
2、Ta 2 O 5 Adding deionized water and octadecylamine ammonium acetate into the powder, and removingIonic water, octadecenylamine ammonium acetate and Ta 2 O 5 The mass ratio of the powder is 50, 0.5 and 1000, preparing slurry with solid content of 50 percent, and grinding the slurry by a sand mill until the particle size of the powder is 0.4 mu m and Ta 2 O 5 The slurry is atomized and granulated, and the particle size of the agglomerated slurry is 90 mu m. The powder is put into a die with the die pressing pressure of 500Kg/cm 2 Keeping the cold isostatic pressure at 270MPa for 10min. A biscuit with a relative density of 70% was obtained. Sintering at 1400 deg.C for 8 hr in pure oxygen atmosphere at normal pressure to obtain Ta with relative density of 99.8% 2 O 5 A ceramic target material.
Example 2:
1. the purity is 4N, the specific surface area is 100m 2 Ta (OH) per g 5 The powder is sequentially calcined at low temperature and high temperature to obtain 25m 2 Ta of specific surface area/g 2 O 5 And (3) powder. Wherein the low-temperature calcination temperature is 750 ℃, and the air atmosphere is kept for 6 hours. The high-temperature calcination temperature is 1200 ℃, the high-temperature calcination time is 8 hours, and the high-temperature calcination atmosphere is an oxygen atmosphere.
2、Ta 2 O 5 Adding deionized water and octadecenylamine ammonium acetate, deionized water, octadecenylamine ammonium acetate and Ta to the powder 2 O 5 The mass ratio of the powder is 65, 1.0 and 100, slurry with the solid content of 65 percent is prepared, and the powder is ground by a sand mill until the particle diameter of the powder is 0.5 mu m and Ta 2 O 5 The slurry is atomized and granulated to have a particle size of 120 μm. Loading the powder into a mold under a molding pressure of 600Kg/cm 2 Keeping the cold isostatic pressure at 300MPa for 20min. A biscuit with a relative density of 65% was obtained. Sintering at 1550 deg.C in pure oxygen atmosphere at normal pressure for 12 hr to obtain Ta with relative density of 99.2% 2 O 5 A ceramic target material.
Example 3:
1. the purity is 4N, the specific surface area is 50m 2 Ta (OH) per g 5 The powder is sequentially calcined at low temperature and high temperature to obtain 5m 2 Ta of specific surface area/g 2 O 5 And (3) powder. Wherein the low-temperature calcination temperature is 600 ℃, and the air atmosphere is kept for 3 hours. The high-temperature calcination temperature is 800 ℃, and the high-temperature calcination is carried outThe time of (2) was 2 hours, and the atmosphere of the high-temperature calcination was an oxygen atmosphere.
2、Ta 2 O 5 Adding deionized water and octadecylamine ammonium acetate, deionized water, octadecylamine ammonium acetate and Ta to the powder 2 O 5 The mass ratio of the powder is 35, 0.1 and 100, slurry with solid content of 35% is prepared, and the powder is ground by a sand mill until the particle size of the powder is 0.3 mu m and Ta 2 O 5 The slurry is atomized and granulated, and the particle size of the agglomerated slurry is 50 microns. Loading the powder into a mold under a molding pressure of 300Kg/cm 2 Keeping the cold isostatic pressure at 240MPa for 5min. A biscuit with a relative density of 63% was obtained. Sintering at 1200 deg.C for 3 hr under normal pressure and pure oxygen atmosphere to obtain Ta with relative density of 99.5% 2 O 5 A ceramic target material.
Example 4:
1. the purity is 4N, the specific surface area is 70m 2 Ta (OH) per g 5 The powder is sequentially calcined at low temperature and high temperature to obtain 10m 2 Ta of specific surface area/g 2 O 5 And (3) powder. Wherein the low-temperature calcination temperature is 650 ℃, and the air atmosphere is kept for 4 hours. The high-temperature calcination temperature is 900 ℃, the high-temperature calcination time is 3 hours, and the high-temperature calcination atmosphere is an oxygen atmosphere.
2、Ta 2 O 5 Adding deionized water and cis-9-octadecenoate, deionized water, cis-9-octadecenoate and Ta to the powder 2 O 5 The mass ratio of the powder is 40, 0.3 and 100, preparing slurry with solid content of 40 percent, and grinding the slurry by a sand mill until the particle size of the powder is 0.5 mu m and Ta 2 O 5 The slurry was atomized and granulated to a particle size of 70 μm. Loading the powder into a mold under a molding pressure of 350Kg/cm 2 Keeping the cold isostatic pressure at 260MPa for 8min. A biscuit with a relative density of 65% was obtained. Sintering at 1300 deg.C for 6 hr under pure oxygen atmosphere at normal pressure to obtain Ta with relative density of 99.4% 2 O 5 A ceramic target material.
Example 5:
1. the purity is 4N, the specific surface area is 90m 2 Ta (OH) per gram 5 The powder is sequentially calcined at low temperature and high temperature to obtain 20m 2 Ta of specific surface area/g 2 O 5 And (3) powder. Wherein the low-temperature calcination temperature is 720 ℃, and the air atmosphere is kept for 4 hours. The high-temperature calcination temperature is 1100 ℃, the high-temperature calcination time is 7 hours, and the high-temperature calcination atmosphere is an oxygen atmosphere.
2、Ta 2 O 5 Adding deionized water and polyethylene glycol 600, deionized water, polyethylene glycol 600 and Ta into the powder 2 O 5 The mass ratio of the powder is 60, 0.8 and 100, preparing slurry with solid content of 60 percent, and grinding the slurry by a sand mill until the particle size of the powder is 0.2 mu m and Ta 2 O 5 The slurry is atomized and granulated, and the particle size of the agglomerated slurry is 110 mu m. The powder is put into a die with the die pressing pressure of 550Kg/cm 2 Keeping the cold isostatic pressure at 280MPa for 18min. A biscuit with a relative density of 70% was obtained. Sintering at 1500 deg.C for 10 hr under normal pressure and pure oxygen atmosphere to obtain Ta with relative density of 99.6% 2 O 5 A ceramic target material.
Although the embodiments of the present invention have been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the embodiments of the present invention.
Claims (9)
1. Ta 2 O 5 The preparation method of the ceramic target is characterized by comprising the following steps:
step one, ta (OH) 5 The powder is sequentially calcined at low temperature and high temperature to obtain Ta 2 O 5 A powder;
the low-temperature calcination temperature is 600-750 ℃, the low-temperature calcination time is 3-6 hours, and the low-temperature calcination atmosphere is air atmosphere;
the high-temperature calcination temperature is 800-1200 ℃, the high-temperature calcination time is 2-8 hours, and the high-temperature calcination atmosphere is oxygen atmosphere;
step two, adding deionized water and a dispersing agent into Ta 2 O 5 In the powder to obtain Ta 2 O 5 Grinding, atomizing, granulating, agglomerating, molding, cold isostatic pressing and sintering in normal-pressure oxygen atmosphere to obtain Ta for coating 2 O 5 A ceramic target material;
in the second step, the deionized water, the dispersant and Ta 2 O 5 The mass ratio of the powder is 35-65, 0.1-1.0 and 100.
2. The method of claim 1, wherein in step one, the Ta (OH) 5 The purity of the powder is 4N, and the specific surface area is 50-100 m 2 /g；
Said Ta 2 O 5 The specific surface area of the powder is 5 to 25m 2 /g。
3. The method according to claim 1, wherein the dispersant is one of octadecenylamine ammonium acetate, cis-9-octadecenoic acid, and polyethylene glycol 600.
4. The method according to any one of claims 1 to 3, wherein in the second step, ta after grinding 2 O 5 The grain diameter of the slurry is less than or equal to 0.5 mu m;
the process conditions of atomization granulation are as follows: the centrifugal rotating speed is 12000-25000 rpm, and the hot air outlet temperature is 100-130 ℃;
agglomerated Ta 2 O 5 The particle size of the slurry is 50-120 mu m.
5. The production method according to any one of claims 1 to 3, wherein in the second step, the pressure of the molding is 300 to 600kg/cm 2 。
6. The production method according to any one of claims 1 to 3, wherein in the second step, the cold isostatic pressing is performed at a pressure of 240 to 300MPa for a dwell time of 5 to 20min.
7. The preparation method according to any one of claims 1 to 3, wherein in the second step, the process conditions of the atmospheric pressure oxygen atmosphere sintering are as follows: the sintering temperature is 1200-1550 ℃, and the heat preservation time is 3-12 hours.
8. The method according to any one of claims 1 to 3, wherein in step two, the Ta 2 O 5 The relative density of the ceramic target material is more than or equal to 99 percent.
9. Ta 2 O 5 A ceramic target material, characterized in that Ta 2 O 5 The ceramic target is obtained by the preparation method of any one of claims 1 to 8.
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| DE10296409B4 (en) * | 2001-12-27 | 2006-06-08 | Mitsui Mining & Smelting Co., Ltd. | Tantalum oxide or niobium oxide powder and process for their preparation |
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