Preparation method of high-tap-density niobium oxide and high-tap-density niobium oxide prepared by same

Abstract

The invention discloses a preparation method of high-tap-density niobium oxide. The preparation method comprises the following steps: neutralization and sedimentation; washing and defluorination; drying; calcining; and sieving, wherein in the neutralization and sedimentation step, a high-purity niobium liquid is neutralized by ammonia gas for 2-4 hours till the pH is equal to 9-10; high-purity niobium hydroxide obtained by washing and defluorination is squeezed for 4-10 hours; high-purity niobium oxide which is calcined and cooled is sieved by a 30-mesh sieve. According to the high-tap-density niobium oxide prepared by the method disclosed by the invention, the tap density is greater than 1.5g / cm<3> and the diameter D50 is equal to 10-12 mu m. According to the high-tap density niobium oxide prepared by the method disclosed by the invention, the shrinking percentage and porosity in the target calcining and forming process are effectively reduced, thereby facilitating target moulding. The sputtering performance of the target is improved.

Description

technical field

[0001] The invention belongs to the field of metal chemical smelting, and specifically relates to a method for preparing niobium oxide with a large tap density and high-purity niobium oxide with a large tap density prepared by the method. Background technique

[0002] Sputtering coating is a new type of physical vapor coating method, which has obvious advantages compared with evaporation coating. The working principle of sputtering coating is: the ions generated by the ion source are accelerated and gathered in a vacuum to form a high-speed energy ion beam, which bombards the solid surface and exchanges kinetic energy with the atoms on the solid surface, so that the atoms on the solid surface leave the solid and fly away. Deposit the film on the substrate and on the surface of the substrate. The solid being bombarded is called a sputtering target.

[0003] Niobium oxide (Nb 2 o 5 ) target as a sputtering target is used in optical interference filters, ele...

Examples

Embodiment 1

[0054] Example 1 Preparation of high-purity niobium oxide with large tap density

[0055] 1. Transfer 1200L high-niobium liquid to the neutralization tank, and after fully stirring for 10 minutes, slowly open the ammonia gas valve to feed ammonia gas, and adjust the ammonia gas pressure for 3 hours to neutralize to pH=9 to obtain high-purity niobium hydroxide Slurry. Among them, with (Ta+Nb) 2 o 5 Calculated, the oxide concentration of high niobium liquid is 140g / L, and the acidity is 5.2N.

[0056] 2. Press the neutralized high-purity niobium hydroxide slurry into a filter press with a washing capacity of 170Kg. After drying, transfer the filter cake into a slurry mixing tank, and then inject ammonia-saturated pure water at 60~70°C for adjustment. Wash, adjust the filter cake into a slurry that can be stirred, and after stirring for 30 minutes, press the slurry into the filter press to dry, repeat the above steps 3 times, and the water discharged by the filter press i...

Embodiment 2

[0061] Example 2 Preparation of high-purity niobium oxide with large tap density

[0062] 1. Transfer 1160L high-niobium liquid to the neutralization tank, and after fully stirring for 20 minutes, slowly open the ammonia gas valve to feed ammonia gas, and adjust the ammonia gas pressure for 3.5 hours to neutralize to pH=10 to obtain high-purity niobium hydroxide Slurry. Among them, with (Ta+Nb) 2 o 5 According to calculation, the oxide concentration of high niobium liquid is 146g / L, and the acidity is 5.3N.

[0063] 2. Press the neutralized high-purity niobium hydroxide slurry into a filter press with a washing capacity of 170Kg. After drying, transfer the filter cake into a slurry mixing tank, and then inject ammonia-saturated pure water at 60~70°C for adjustment. Wash, adjust the filter cake into a slurry that can be stirred, and after stirring for 50 minutes, press the slurry into the filter press to dry, repeat the above steps 3 times, and the water discharged by ...

Embodiment 3

[0068] Example 3 Preparation of high-purity niobium oxide with large tap density

[0069] 1. Transfer 1000L high-niobium liquid to the neutralization tank, and after fully stirring for 5 minutes, slowly open the ammonia gas valve to feed ammonia gas, and adjust the ammonia gas pressure for 2 hours to neutralize to pH=9 to obtain high-purity niobium hydroxide Slurry. Among them, with (Ta+Nb) 2 o 5 Calculated, the oxide concentration of high niobium liquid is 130g / L, and the acidity is 5.0N.

[0070] 2. Press the neutralized high-purity niobium hydroxide slurry into a filter press with a washing capacity of 170Kg. After drying, transfer the filter cake into a slurry mixing tank, and then inject ammonia-saturated pure water at 60~70°C for adjustment. Wash, adjust the filter cake into a slurry that can be stirred, and after stirring for 20 minutes, press the slurry into the filter press to dry, repeat the above steps 3 times, and the water discharged by the filter press i...

technical field

[0001] The invention belongs to the field of metal chemical smelting, and specifically relates to a method for preparing niobium oxide with a large tap density and high-purity niobium oxide with a large tap density prepared by the method. Background technique

[0002] Sputtering coating is a new type of physical vapor coating method, which has obvious advantages compared with evaporation coating. The working principle of sputtering coating is: the ions generated by the ion source are accelerated and gathered in a vacuum to form a high-speed energy ion beam, which bombards the solid surface and exchanges kinetic energy with the atoms on the solid surface, so that the atoms on the solid surface leave the solid and fly away. Deposit the film on the substrate and on the surface of the substrate. The solid being bombarded is called a sputtering target.

[0003] Niobium oxide (Nb 2 o 5 ) target as a sputtering target is used in optical interference filters, ele...

Examples

Embodiment 1

[0054] Example 1 Preparation of high-purity niobium oxide with large tap density

[0055] 1. Transfer 1200L high-niobium liquid to the neutralization tank, and after fully stirring for 10 minutes, slowly open the ammonia gas valve to feed ammonia gas, and adjust the ammonia gas pressure for 3 hours to neutralize to pH=9 to obtain high-purity niobium hydroxide Slurry. Among them, with (Ta+Nb) 2 o 5 Calculated, the oxide concentration of high niobium liquid is 140g / L, and the acidity is 5.2N.

[0056] 2. Press the neutralized high-purity niobium hydroxide slurry into a filter press with a washing capacity of 170Kg. After drying, transfer the filter cake into a slurry mixing tank, and then inject ammonia-saturated pure water at 60~70°C for adjustment. Wash, adjust the filter cake into a slurry that can be stirred, and after stirring for 30 minutes, press the slurry into the filter press to dry, repeat the above steps 3 times, and the water discharged by the filter press i...

Embodiment 2

[0061] Example 2 Preparation of high-purity niobium oxide with large tap density

[0062] 1. Transfer 1160L high-niobium liquid to the neutralization tank, and after fully stirring for 20 minutes, slowly open the ammonia gas valve to feed ammonia gas, and adjust the ammonia gas pressure for 3.5 hours to neutralize to pH=10 to obtain high-purity niobium hydroxide Slurry. Among them, with (Ta+Nb) 2 o 5 According to calculation, the oxide concentration of high niobium liquid is 146g / L, and the acidity is 5.3N.

[0063] 2. Press the neutralized high-purity niobium hydroxide slurry into a filter press with a washing capacity of 170Kg. After drying, transfer the filter cake into a slurry mixing tank, and then inject ammonia-saturated pure water at 60~70°C for adjustment. Wash, adjust the filter cake into a slurry that can be stirred, and after stirring for 50 minutes, press the slurry into the filter press to dry, repeat the above steps 3 times, and the water discharged by ...

Embodiment 3

[0068] Example 3 Preparation of high-purity niobium oxide with large tap density

[0069] 1. Transfer 1000L high-niobium liquid to the neutralization tank, and after fully stirring for 5 minutes, slowly open the ammonia gas valve to feed ammonia gas, and adjust the ammonia gas pressure for 2 hours to neutralize to pH=9 to obtain high-purity niobium hydroxide Slurry. Among them, with (Ta+Nb) 2 o 5 Calculated, the oxide concentration of high niobium liquid is 130g / L, and the acidity is 5.0N.

[0070] 2. Press the neutralized high-purity niobium hydroxide slurry into a filter press with a washing capacity of 170Kg. After drying, transfer the filter cake into a slurry mixing tank, and then inject ammonia-saturated pure water at 60~70°C for adjustment. Wash, adjust the filter cake into a slurry that can be stirred, and after stirring for 20 minutes, press the slurry into the filter press to dry, repeat the above steps 3 times, and the water discharged by the filter press i...