CN111606708A - Low-resistivity niobium pentoxide hot-pressing target material and preparation method thereof - Google Patents
Low-resistivity niobium pentoxide hot-pressing target material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a low-resistivity niobium pentoxide hot-pressing target material and a preparation method thereof, belonging to the technical field of coating materials. The method comprises the steps of performing vacuum pre-sintering on a mixture of niobium pentoxide powder and niobium powder, reacting part of niobium pentoxide with niobium to generate niobium monoxide and niobium dioxide, generating niobium dioxide from the niobium pentoxide in a vacuum oxygen-loss state to obtain niobium oxide containing the niobium monoxide, and performing hot-press sintering to obtain the niobium pentoxide hot-press target with higher density. The niobium pentoxide hot-pressing target material contains a niobium monoxide conductor and a niobium dioxide semiconductor, so that the resistivity of the target material is effectively reduced, and the conductivity is improved.
Description
Technical Field
The invention relates to the technical field of coating materials, in particular to a low-resistivity niobium pentoxide hot-pressing target material and a preparation method thereof.
Background
The niobium pentoxide hot-pressing target material is widely used for optical sputtering coating, has good optical performance, and is widely used for front cover glass and rear cover glass of mobile phones and tablet computers, the niobium pentoxide plated on the front cover glass is used as an antireflection film to increase the transmittance of products, and the niobium pentoxide plated on the rear cover glass is used for adjusting the color of the glass and plating colorful rear covers with different colors.
The existing niobium pentoxide target is mainly obtained by hot-pressing niobium pentoxide powder in vacuum, and the principle is that the niobium pentoxide forms NbO under the high-vacuum oxygen loss state2However, the target material prepared by the method has high resistivity and poor conductivity, and is easy to generate nodules in the use process to influence the performance of the film.
Disclosure of Invention
The invention aims to provide a niobium pentoxide hot-pressing target material with low resistivity and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a low-resistivity niobium pentoxide hot-pressing target material, which comprises the following steps:
mixing niobium pentoxide powder and niobium powder, and performing vacuum pre-sintering to obtain niobium oxide containing niobium monoxide;
and carrying out ball milling on the niobium oxide containing the niobium monoxide, and carrying out hot-pressing sintering to obtain the low-resistivity niobium pentoxide hot-pressing target material.
Preferably, the mass ratio of the niobium pentoxide powder to the niobium powder is 100: 1-5.
Preferably, the temperature of the vacuum pre-sintering is 1200-1400 ℃, the absolute pressure is less than or equal to 0.1Pa, and the time is 3-8 h.
Preferably, the temperature rising rate from room temperature to the vacuum pre-sintering temperature is 1-8 ℃/min.
Preferably, the hot-pressing sintering temperature is 1200-1450 ℃, the pressure is 130-170 t, and the heat preservation and pressure maintaining time is 5-13 h.
Preferably, the temperature rising rate from room temperature to the hot-pressing sintering temperature is 1-7 ℃/min, and the pressure rising rate from pressureless pressure rising to the hot-pressing sintering pressure is 1-10 t/min.
Preferably, the particle size of the niobium powder and the niobium pentoxide powder is independently less than or equal to 0.05 mm.
Preferably, the mixing comprises mechanical vibratory screening and blender mixing in sequence; the mechanical vibration screen is used for screening through a 35-mesh screen, a 60-mesh screen, an 80-mesh screen, a 100-mesh screen and a 120-mesh screen from top to bottom in sequence; the mixing speed of the mixer is 15-30 rpm, and the mixing time is 2-8 h.
Preferably, the ball diameter of the grinding balls used for ball milling is 5-40 mm, the ball-material ratio is 1: 1-2, the rotation speed of ball milling is 10-25 rpm, and the ball milling time is 1-6 h.
The invention also provides the low-resistivity niobium pentoxide hot-pressing target material prepared by the preparation method in the technical scheme, and the low-resistivity niobium pentoxide hot-pressing target material comprises niobium monoxide and niobium dioxide.
The invention provides a preparation method of a low-resistivity niobium pentoxide hot-pressed target material, which comprises the steps of carrying out vacuum pre-sintering on a mixture of niobium pentoxide powder and niobium powder, reacting part of niobium pentoxide with niobium to generate niobium monoxide and niobium dioxide, generating niobium dioxide by the niobium pentoxide in a vacuum oxygen loss state to obtain niobium oxide containing the niobium monoxide, and carrying out hot-pressed sintering to obtain the niobium pentoxide hot-pressed target material with higher density. The niobium pentoxide hot-pressing target material contains a niobium monoxide conductor and a niobium dioxide semiconductor, so that the resistivity of the target material is effectively reduced, and the conductivity is improved.
Detailed Description
The invention provides a preparation method of a low-resistivity niobium pentoxide hot-pressing target material, which comprises the following steps:
mixing niobium pentoxide powder and niobium powder, and performing vacuum pre-sintering to obtain niobium oxide containing niobium monoxide;
and carrying out ball milling on the niobium oxide containing the niobium monoxide, and carrying out hot-pressing sintering to obtain the low-resistivity niobium pentoxide hot-pressing target material.
The niobium pentoxide powder and the niobium powder are mixed and then subjected to vacuum pre-sintering to obtain niobium oxide containing niobium monoxide.
In the invention, the mass ratio of the niobium pentoxide powder to the niobium powder is preferably 100:1 to 5, and more preferably 100:3 to 4. In the invention, the ratio of the niobium powder is too small, so that the resistivity of the obtained niobium pentoxide target material is too high, and the process parameters are required to be adjusted to a greater degree when the content of the niobium pentoxide target material is too high, and the ratio can ensure lower resistivity and carry out film coating under the condition of the original niobium oxide film coating.
In the present invention, the niobium powder preferably has a particle size of 0.05mm or less (i.e., 300 mesh), more preferably 0.045mm or less (i.e., 325 mesh), and a purity of 99.95%; the granularity of the niobium pentoxide powder is preferably less than or equal to 0.05mm (namely 300 meshes), and the purity is preferably 99.95%; the mixing preferably comprises mechanical vibration screen sieving and mixer mixing which are sequentially carried out; the mechanical vibration screen is preferably used for screening through a 35-mesh screen, a 60-mesh screen, an 80-mesh screen, a 100-mesh screen and a 120-mesh screen from top to bottom in sequence; the mixing speed of the mixer is preferably 15-30 rpm, more preferably 20-25 rpm, the time is preferably 2-8 h, more preferably 5-6 h, the type of the mixer is not particularly limited, a V-shaped mixer is preferably used in the embodiment of the invention, and the powder filling amount of the V-shaped mixer is preferably not more than 2/3. In the invention, the sieving of the mechanical vibration screen can not only disperse the niobium pentoxide powder and the niobium powder, but also fully mix the niobium pentoxide powder and the niobium powder; the mixing of the blender mixer can further mix the niobium pentoxide powder and the niobium powder evenly.
Preferably, the mixture obtained by mixing is placed in a graphite crucible, and then the graphite crucible is placed in a vacuum furnace for vacuum pre-sintering; for filling a plurality of mixtures, the mixtures are preferably placed in a graphite crucible and then compacted; in order to ensure that the oxygen is sufficiently lost in the vacuum pre-sintering process, a plurality of small holes are preferably inserted in the compacted mixture, the diameter of each small hole is preferably 2mm, the interval is preferably 2-5 cm, and more preferably 2.5-5 cm.
In the invention, the temperature of the vacuum pre-sintering is preferably 1200-1400 ℃, more preferably 1270-1300 ℃, the absolute pressure is preferably less than or equal to 0.1Pa, and the time is preferably 3-8 h, more preferably 3-5 h; the heating rate from the room temperature to the vacuum pre-sintering temperature is preferably 1-8 ℃/min, and more preferably 3-5 ℃/min; after the vacuum pre-sintering is completed, the product obtained by the vacuum pre-sintering is preferably cooled to room temperature along with the furnace. In the invention, the niobium powder reacts with part of niobium pentoxide to generate niobium monoxide and niobium dioxide in the vacuum pre-sintering process, and simultaneously the niobium pentoxide is subjected to vacuum oxygen loss to generate niobium dioxide.
After the niobium oxide containing niobium monoxide is obtained, the niobium oxide containing niobium monoxide is subjected to ball milling and hot-pressing sintering to obtain the low-resistivity niobium pentoxide hot-pressing target material.
In the invention, the oxide of niobium containing niobium monoxide is sieved by a sieve with 80-120 meshes before ball milling, and the sieve with 80 meshes, 100 meshes or 120 meshes can be particularly preferred. In the invention, the sieving can refine the powder, avoid agglomeration, make the NbO powder in the powder more dispersed, and make the resistivity of the obtained target material stable.
In the invention, the ball diameter (diameter) of the grinding balls used for ball milling is preferably 5-40 mm, and more preferably 20-35 mm; the ball-to-material ratio of the ball milling is preferably 1: 1-2, and more preferably 1: 1-1.5; the rotation speed of the ball milling is preferably 10-25 rpm, and more preferably 15-20 rpm; the ball milling time is preferably 1-6 h, and more preferably 3-6 h. The material of the grinding ball is not particularly limited, and the grinding ball can be any conventional grinding ball, such as a polished alumina ball.
In the invention, the temperature of the hot-pressing sintering is preferably 1200-1450 ℃, and more preferably 1250-1300 ℃; the pressure of the hot-pressing sintering is preferably 130-170 t (ton), and more preferably 140-160 t; the heat preservation and pressure maintaining time of the hot-pressing sintering is preferably 5-13 h, and more preferably 8-10 h; the heating rate from room temperature to the hot-pressing sintering temperature is preferably 1-7 ℃/min, more preferably 2.5-5 ℃/min, and the pressure increasing rate from non-pressure increasing to the hot-pressing sintering pressure is preferably 1-10 t/min, more preferably 2-5 t/min; the temperature rise and the pressure rise are preferably carried out simultaneously; after the hot-pressing sintering is completed, the furnace is preferably cooled to room temperature. In the invention, the hot-pressing sintering can be used for hot-pressing sintering the mixture obtained by ball milling into the high-density target material.
The mould used for the hot-pressing sintering is not specially limited, and a conventional hot-pressing sintering mould, such as an isostatic pressing graphite mould, is adopted.
Those skilled in the art can select a suitable mold or perform machining (e.g., electrical discharge cutting, surface grinding, fine engraving and other equipment machining) as required to obtain a target material with a suitable specification.
The invention also provides the low-resistivity niobium pentoxide hot-pressing target material prepared by the preparation method in the technical scheme, which comprises the components of niobium monoxide and niobium dioxide; the density of the low-resistivity niobium pentoxide hot-pressing target material is preferably more than or equal to 4.5g/cm3More preferably 4.53 to 4.56g/cm3(ii) a The resistivity of the low-resistivity niobium pentoxide hot-pressing target is preferably less than or equal to 0.04 omega-cm, and more preferably 0.0364-0.0385 omega-cm; the purity of the low-resistivity niobium pentoxide hot-pressing target (namely, the mass percentage of niobium and oxygen in the low-resistivity niobium pentoxide target) is preferably more than or equal to 99.95%.
The present invention provides a low resistivity niobium pentoxide hot-pressed target material and a method for preparing the same, which are described in detail below with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Mixing niobium pentoxide powder (300 meshes, purity 99.95%) and niobium powder (325 meshes, purity 99.95%) according to a mass ratio of 100:4, sequentially sieving the niobium pentoxide powder and the niobium powder by mechanical vibration screens of 35 meshes, 60 meshes, 80 meshes, 100 meshes and 120 meshes, and mixing the obtained mixture for 5 hours by using a V-shaped mixer, wherein the filling amount of the mixture is not more than 2/3 of the V-shaped mixer, and the rotating speed is 22rpm, so as to obtain a uniformly mixed mixture; putting the uniformly mixed mixture into a graphite crucible, compacting, then inserting small holes in the compacted mixture at a distance of 3cm from each other on a quartz rod with the diameter of 2mm, putting the mixture into a vacuum furnace, vacuumizing to an absolute pressure below 0.1Pa, heating to 1270 ℃ at the speed of 3 ℃/min, preserving heat for 5 hours, and cooling to room temperature along with the furnace to obtain niobium oxide containing niobium monoxide;
sieving the niobium oxide containing niobium monoxide by a 120-mesh sieve, putting the undersize into a ball milling tank, taking a polished alumina ball with the ball diameter of 30mm as a grinding ball, ball milling for 3h at the rotating speed of 20rpm at the ball-material ratio of 1:1.5, putting the ball milled for 3h into a graphite mold, putting the graphite mold into a hot-pressing sintering furnace, increasing the pressure to 140t at the pressure increasing speed of 2t/min, simultaneously increasing the temperature to 1300 ℃ at the temperature increasing speed of 3 ℃/min, preserving the heat and maintaining the pressure for 10h, and then cooling the graphite mold to room temperature to obtain the low-resistivity niobium pentoxide hot-pressing target material.
Example 2
Mixing niobium pentoxide powder (300 meshes, purity 99.95%) and niobium powder (325 meshes, purity 99.95%) according to a mass ratio of 100:3.5, sequentially sieving by mechanical vibration screens of 35 meshes, 60 meshes, 80 meshes, 100 meshes and 120 meshes, and mixing the obtained mixture by a V-shaped mixer for 6 hours, wherein the filling amount of the mixture is not more than 2/3 of the V-shaped mixer, and the rotating speed is 20rpm, so as to obtain a uniformly mixed mixture; putting the uniformly mixed mixture into a graphite crucible, compacting, then inserting small holes in the compacted mixture at a distance of 2.5cm from each other on a quartz rod with the diameter of 2mm, putting the mixture into a vacuum furnace, vacuumizing to an absolute pressure below 0.1Pa, heating to 1300 ℃ at the speed of 3 ℃/min, preserving heat for 4h, and cooling to room temperature along with the furnace to obtain niobium oxide containing niobium monoxide;
and (2) sieving the niobium oxide containing the niobium monoxide by a 100-mesh sieve, putting the sieved material into a ball milling tank, taking a polished alumina ball with the ball diameter of 35mm as a grinding ball, ball milling for 5 hours at a rotating speed of 20rpm at a ball-to-material ratio of 1:1, putting the ball milled material into a graphite mold, putting the graphite mold into a hot-pressing sintering furnace, increasing the pressure to 150t at a pressure increasing speed of 1.5t/min, simultaneously increasing the temperature to 1260 ℃ at a temperature increasing speed of 2.5 ℃/min, preserving the temperature and the pressure for 9 hours, and then cooling the material to room temperature along with the furnace to obtain the low-resistivity niobium pentoxide hot-pressing target material.
Example 3
Mixing niobium pentoxide powder (300 meshes, purity 99.95%) and niobium powder (300 meshes, purity 99.95%) according to a mass ratio of 100:3, sequentially sieving the mixture by 35-mesh, 60-mesh, 80-mesh, 100-mesh and 120-mesh mechanical vibration screens, and mixing the obtained mixture for 6 hours by using a V-shaped mixer, wherein the filling amount of the mixture is not more than 2/3 of the V-shaped mixer, and the rotating speed is 25rpm, so as to obtain a uniformly mixed mixture; putting the uniformly mixed mixture into a graphite crucible, compacting, then inserting small holes in the compacted mixture at a distance of 5cm from each other on a quartz rod with the diameter of 2mm, putting the mixture into a vacuum furnace, vacuumizing to an absolute pressure below 0.1Pa, heating to 1300 ℃ at a speed of 5 ℃/min, preserving heat for 3h, and cooling to room temperature along with the furnace to obtain niobium oxide containing niobium monoxide;
sieving the niobium oxide containing niobium monoxide by a sieve of 80 meshes, putting the undersize into a ball milling tank, taking a polished alumina ball with the ball diameter of 20mm as a grinding ball, ball milling for 6h at the rotating speed of 15rpm at the ball-material ratio of 1:1, putting the ball milled for 6h into a graphite mold, putting the graphite mold into a hot-pressing sintering furnace, increasing the pressure to 160t at the pressure increasing speed of 5t/min, simultaneously increasing the temperature to 1250 ℃ at the temperature increasing speed of 5 ℃/min, preserving the heat and maintaining the pressure for 8h, and then cooling the material to room temperature along with the furnace to obtain the low-resistivity niobium pentoxide hot-pressing target material.
The densities of the targets obtained in examples 1 to 3 were measured by a drainage method, the resistivities of the targets obtained in examples 1 to 3 were measured by a four-probe resistivity tester, and the purities of the targets obtained in examples 1 to 3 were measured by ICP-MS, with the results shown in table 1. As can be seen from table 1, the target material obtained by the preparation method provided by the present invention has high purity and density, low resistivity, and good conductivity.
TABLE 1 Performance test results of low resistivity niobium pentoxide target materials obtained in examples 1-3
| Serial number | Density (g/cm)3) | Resistivity (omega cm) | Purity (%) |
| Example 1 | 4.56 | 0.0365 | 99.95 |
| Example 2 | 4.53 | 0.0385 | 99.95 |
| Example 3 | 4.54 | 0.0364 | 99.95 |
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the low-resistivity niobium pentoxide hot-pressed target material is characterized by comprising the following steps of:
mixing niobium pentoxide powder and niobium powder, and performing vacuum pre-sintering to obtain niobium oxide containing niobium monoxide;
and carrying out ball milling on the niobium oxide containing the niobium monoxide, and carrying out hot-pressing sintering to obtain the low-resistivity niobium pentoxide hot-pressing target material.
2. The production method according to claim 1, wherein the mass ratio of the niobium pentoxide powder to the niobium powder is 100:1 to 5.
3. The preparation method according to claim 1 or 2, wherein the temperature of the vacuum pre-sintering is 1200-1400 ℃, the absolute pressure is less than or equal to 0.1Pa, and the time is 3-8 h.
4. The method according to claim 3, wherein a temperature rise rate from room temperature to the vacuum pre-sintering temperature is 1 to 8 ℃/min.
5. The preparation method according to claim 1 or 2, wherein the hot-pressing sintering temperature is 1200-1450 ℃, the pressure is 130-170 t, and the holding time is 5-13 h.
6. The production method according to claim 5, wherein a temperature rise rate from room temperature to the temperature of the hot press sintering is 1 to 7 ℃/min, and a pressure rise rate from pressureless pressure rise to the pressure of the hot press sintering is 1 to 10 t/min.
7. The production method according to claim 1 or 2, wherein the niobium powder and the niobium pentoxide powder have a particle diameter of 0.05mm or less, independently.
8. The method of claim 7, wherein the mixing comprises mechanical vibratory screening and blender mixing in sequence; the mechanical vibration screen is used for screening through a 35-mesh screen, a 60-mesh screen, an 80-mesh screen, a 100-mesh screen and a 120-mesh screen from top to bottom in sequence; the mixing speed of the mixer is 15-30 rpm, and the mixing time is 2-8 h.
9. The preparation method of claim 1, wherein the ball diameter of the grinding balls used for ball milling is 5-40 mm, the ball-to-material ratio is 1: 1-2, the rotation speed of ball milling is 10-25 rpm, and the ball milling time is 1-6 h.
10. The low-resistivity niobium pentoxide hot-pressed target material prepared by the preparation method of any one of claims 1 to 9 comprises niobium monoxide and niobium dioxide.
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