阅读说明：本技术 一种基于真空溅射腔室的贵金属回收工艺 (Noble metal recovery process based on vacuum sputtering chamber ) 是由 陈敏 周鑫 郭丽萍 于 2020-12-21 设计创作，主要内容包括：本发明属于钼片技术领域,具体涉及一种基于真空溅射腔室的贵金属回收工艺,包括步骤1,将防着板全部浸入硝酸溶液中；步骤2,将防着板浸入电解溶液中；步骤3,将防着板浸入氢氟酸溶液中；步骤4,将防着板放入喷砂机中喷砂处理,完成防着板处理；步骤5,将步骤1和2中的溶液用过滤纱布过滤出沉淀或固体状钌；步骤6,将滤出的沉淀或固体钌再次浸入硝酸溶液中；步骤7,将步骤6中的溶液再次使用过滤纱布过滤,然后烘干即可得到金属钌。本发明不仅使得镀膜腔室处于干净清洁的状态,杜绝腔室被污染镀层被污染的可能性,同时可回收贵金属钌,提高效益减少浪费,减少对环境的污染。(The invention belongs to the technical field of molybdenum sheets, and particularly relates to a noble metal recovery process based on a vacuum sputtering chamber, which comprises the following steps of 1, completely immersing a prevention plate in a nitric acid solution; step 2, immersing the anti-sticking plate into an electrolytic solution; step 3, immersing the anti-sticking plate into hydrofluoric acid solution; step 4, putting the anti-sticking plate into a sand blasting machine for sand blasting treatment to finish the anti-sticking plate treatment; step 5, filtering the solution obtained in the step 1 and the step 2 by using a filter gauze to filter out precipitate or solid ruthenium; step 6, immersing the filtered precipitate or solid ruthenium into nitric acid solution again; and 7, filtering the solution obtained in the step 6 by using filter gauze again, and drying to obtain the ruthenium metal. The invention not only ensures that the coating chamber is in a clean state, and the possibility that the chamber is polluted by a polluted coating is avoided, but also can recover the noble metal ruthenium, thereby improving the benefit, reducing the waste and reducing the pollution to the environment.)

1. A noble metal recovery process based on a vacuum sputtering chamber is characterized in that: the method comprises the following steps:

step 1, completely immersing a prevention plate in a nitric acid solution;

step 2, immersing the anti-sticking plate into an electrolytic solution;

step 3, immersing the anti-sticking plate into hydrofluoric acid solution;

step 4, putting the anti-sticking plate into a sand blasting machine for sand blasting treatment to finish the anti-sticking plate treatment;

step 5, filtering the solution obtained in the step 1 and the step 2 by using a filter gauze to filter out precipitate or solid ruthenium;

step 6, immersing the filtered precipitate or solid ruthenium into nitric acid solution again;

and 7, filtering the solution obtained in the step 6 by using filter gauze again, and drying to obtain the ruthenium metal.

2. The vacuum sputtering chamber based precious metal recovery process of claim 1, wherein: the concentration ratio of the nitric acid solution in the step 1 is that 68 percent nitric acid and pure water are mixed in a ratio of 1:1, the soaking time is mainly that the silver layer is completely peeled off, the time is as long as possible, and the nitric acid needs to be supplemented in the middle.

3. The vacuum sputtering chamber based precious metal recovery process of claim 1, wherein: and 2, adopting a mixed alkali liquor as the electrolyte in the electrolytic cell in the step 2, wherein the mixed alkali liquor is formed by mixing a sodium hydroxide solution, sodium bicarbonate and a sodium carbonate solution, the concentration of sodium hydroxide in the mixed alkali liquor is 10-20g/L, the concentration of sodium bicarbonate is 10-20g/L, the concentration of sodium carbonate is 10-20g/L, the electrolytic voltage is 60 volts, and the current is 6 amperes.

4. The vacuum sputtering chamber based precious metal recovery process of claim 1, wherein: the concentration ratio of the hydrofluoric acid solution in the step 3 is formed by mixing experimental hydrofluoric acid and pure water in a ratio of 1:10, the soaking time is 10-20 seconds, and the reaction is carried out on the surface of the titanium plate.

5. The vacuum sputtering chamber based precious metal recovery process of claim 1, wherein: the sand blasting treatment in the step 4 makes the surface roughness of the titanium plate larger, and the molybdenum sheet can be prevented from sliding when placed on the upper surface.

6. The vacuum sputtering chamber based precious metal recovery process of claim 1, wherein: the filtering gauze in the step 5 is normal filtering gauze which can filter the precipitated ruthenium or ruthenium hydroxide in the solution.

7. The vacuum sputtering chamber based precious metal recovery process of claim 1, wherein: the concentration ratio of the nitric acid solution in the step 6 is that the nitric acid solution is formed by mixing 68% nitric acid and pure water in a ratio of 1:1, and the time is as long as possible.

8. The vacuum sputtering chamber based precious metal recovery process of claim 1, wherein: the drying temperature in the step 7 is 100 ℃, and the time is the drying of the precipitate.

Technical Field

The invention belongs to the technical field of molybdenum sheets, and particularly relates to a noble metal recovery process based on a vacuum sputtering chamber.

Background

After magnetron sputtering coating, not only a product is coated, but also a coating is sputtered in a chamber of the whole coating machine, and usually a layer of anti-sticking plate is arranged around the inner wall of the chamber to prevent the sputtered coating from polluting the whole chamber. The anti-adhesion plate has the characteristic of detachable cleaning. In the actual production process, the anti-sticking plate is made of pure titanium, and the plating layer mainly comprises ruthenium and silver, wherein the ruthenium accounts for more than 70%, the silver accounts for more than 25%, and other metals account for less than 5%. The anti-sticking plate needs to be cleaned at regular time to ensure that the coating chamber is clean and pollution-free. However, if the plating layer on the shielding plate is directly removed, the cost is greatly increased, and the heavy metal pollution problem is caused to the environment.

Disclosure of Invention

Aiming at the problems in the prior art, the invention provides a precious metal recovery process based on a vacuum sputtering chamber, which not only enables a coating chamber to be in a clean state and prevents the possibility that the chamber is polluted by a polluted coating, but also can recover precious metal ruthenium, thereby improving the benefit, reducing the waste and reducing the pollution to the environment.

In order to achieve the technical purpose, the technical scheme of the invention is as follows:

a precious metal recovery process based on a vacuum sputtering chamber comprises the following steps:

step 1, completely immersing a prevention plate in a nitric acid solution;

step 2, immersing the anti-sticking plate into an electrolytic solution;

step 3, immersing the anti-sticking plate into hydrofluoric acid solution;

step 4, putting the anti-sticking plate into a sand blasting machine for sand blasting treatment to finish the anti-sticking plate treatment;

step 5, filtering the solution obtained in the step 1 and the step 2 by using a filter gauze to filter out precipitate or solid ruthenium;

step 6, immersing the filtered precipitate or solid ruthenium into nitric acid solution again;

and 7, filtering the solution obtained in the step 6 by using filter gauze again, and drying to obtain the ruthenium metal.

The concentration ratio of the nitric acid solution in the step 1 is that 68 percent nitric acid and pure water are mixed in a ratio of 1:1, the soaking time is mainly that the silver layer is completely peeled off, the time is as long as possible, and the nitric acid needs to be supplemented in the middle.

And 2, adopting a mixed alkali liquor as the electrolyte in the electrolytic cell in the step 2, wherein the mixed alkali liquor is formed by mixing a sodium hydroxide solution, sodium bicarbonate and a sodium carbonate solution, the concentration of sodium hydroxide in the mixed alkali liquor is 10-20g/L, the concentration of sodium bicarbonate is 10-20g/L, and the concentration of sodium carbonate is 10-20 g/L. The electrolysis voltage was 60 volts and the current was 6 amps.

The concentration ratio of the hydrofluoric acid solution in the step 3 is formed by mixing experimental hydrofluoric acid and pure water in a ratio of 1:10, the soaking time is 10-20 seconds, and the reaction is carried out on the surface of the titanium plate.

The sand blasting treatment in the step 4 makes the surface roughness of the titanium plate larger, and the molybdenum sheet can be prevented from sliding when placed on the upper surface.

The filtering gauze in the step 5 is normal filtering gauze which can filter precipitated ruthenium or ruthenium hydroxide and the like in the solution.

The concentration ratio of the nitric acid solution in the step 6 is that the nitric acid solution is formed by mixing 68% nitric acid and pure water in a ratio of 1:1, and the time is as long as possible.

The drying temperature in the step 7 is 100 ℃, and the time is the drying of the precipitate.

The plating layer on the anti-sticking plate is formed by stacking a ruthenium layer, a silver layer, a ruthenium layer and a silver layer in such a way that the ruthenium layer is thicker at individual places, silver is easy to melt in nitric acid, and ruthenium and titanium do not react with the nitric acid, so that the silver is removed and the plating layer is loosened as much as possible by soaking in the nitric acid. And then, putting the titanium plate into hydrofluoric acid, reacting titanium with the hydrofluoric acid, and stripping off a layer of titanium on the surface to ensure that the titanium plate is cleaner. Then ruthenium precipitate in the nitric acid pool and the electrolytic cell is collected and dried for recovery.

From the above description, it can be seen that the present invention has the following advantages:

the invention not only ensures that the coating chamber is in a clean state, and the possibility that the chamber is polluted by a polluted coating is avoided, but also can recover the noble metal ruthenium, thereby improving the benefit, reducing the waste and reducing the pollution to the environment.

Detailed Description

The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.

Example 1

A precious metal recovery process based on a vacuum sputtering chamber comprises the following steps:

step 1, completely immersing a prevention plate in a nitric acid solution;

step 2, immersing the anti-sticking plate into an electrolytic solution;

step 3, immersing the anti-sticking plate into hydrofluoric acid solution;

step 4, putting the anti-sticking plate into a sand blasting machine for sand blasting treatment to finish the anti-sticking plate treatment;

step 5, filtering the solution obtained in the step 1 and the step 2 by using a filter gauze to filter out precipitate or solid ruthenium;

step 6, immersing the filtered precipitate or solid ruthenium into nitric acid solution again;

and 7, filtering the solution obtained in the step 6 by using filter gauze again, and drying to obtain the ruthenium metal.

The concentration ratio of the nitric acid solution in the step 1 is that 68 percent nitric acid and pure water are mixed in a ratio of 1:1, the soaking time is mainly that the silver layer is completely peeled off, the time is as long as possible, and the nitric acid needs to be supplemented in the middle.

And 2, adopting a mixed alkali liquor as the electrolyte in the electrolytic cell in the step 2, wherein the mixed alkali liquor is formed by mixing a sodium hydroxide solution, sodium bicarbonate and a sodium carbonate solution, and the concentration of sodium hydroxide, the concentration of sodium bicarbonate and the concentration of sodium carbonate in the mixed alkali liquor are respectively 10g/L, 10g/L and 10 g/L. The electrolysis voltage was 60 volts and the current was 6 amps.

The concentration ratio of the hydrofluoric acid solution in the step 3 is formed by mixing experimental hydrofluoric acid and pure water in a ratio of 1:10, the soaking time is 10 seconds, and the reaction is carried out on the surface of the titanium plate.

The sand blasting treatment in the step 4 makes the surface roughness of the titanium plate larger, and the molybdenum sheet can be prevented from sliding when placed on the upper surface.

The filtering gauze in the step 5 is normal filtering gauze which can filter precipitated ruthenium or ruthenium hydroxide and the like in the solution.

The concentration ratio of the nitric acid solution in the step 6 is that the nitric acid solution is formed by mixing 68% nitric acid and pure water in a ratio of 1:1, and the time is as long as possible.

The drying temperature in the step 7 is 100 ℃, and the time is the drying of the precipitate.

In this example, the recovery rate of ruthenium metal was 99.6%, and the recovery rate of silver metal was 99.5%.

Example 2

A precious metal recovery process based on a vacuum sputtering chamber comprises the following steps:

step 1, completely immersing a prevention plate in a nitric acid solution;

step 2, immersing the anti-sticking plate into an electrolytic solution;

step 3, immersing the anti-sticking plate into hydrofluoric acid solution;

step 4, putting the anti-sticking plate into a sand blasting machine for sand blasting treatment to finish the anti-sticking plate treatment;

step 5, filtering the solution obtained in the step 1 and the step 2 by using a filter gauze to filter out precipitate or solid ruthenium;

step 6, immersing the filtered precipitate or solid ruthenium into nitric acid solution again;

and 7, filtering the solution obtained in the step 6 by using filter gauze again, and drying to obtain the ruthenium metal.

The concentration ratio of the nitric acid solution in the step 1 is that 68 percent nitric acid and pure water are mixed in a ratio of 1:1, the soaking time is mainly that the silver layer is completely peeled off, the time is as long as possible, and the nitric acid needs to be supplemented in the middle.

And 2, adopting a mixed alkali liquor as the electrolyte in the electrolytic cell in the step 2, wherein the mixed alkali liquor is formed by mixing a sodium hydroxide solution, sodium bicarbonate and a sodium carbonate solution, and the concentration of sodium hydroxide, the concentration of sodium bicarbonate and the concentration of sodium carbonate in the mixed alkali liquor are respectively 20g/L, 20g/L and 20 g/L. The electrolysis voltage was 60 volts and the current was 6 amps.

The concentration ratio of the hydrofluoric acid solution in the step 3 is formed by mixing experimental hydrofluoric acid and pure water in a ratio of 1:10, the soaking time is 10-20 seconds, and the reaction is carried out on the surface of the titanium plate.

The sand blasting treatment in the step 4 makes the surface roughness of the titanium plate larger, and the molybdenum sheet can be prevented from sliding when placed on the upper surface.

The filtering gauze in the step 5 is normal filtering gauze which can filter precipitated ruthenium or ruthenium hydroxide and the like in the solution.

The concentration ratio of the nitric acid solution in the step 6 is that the nitric acid solution is formed by mixing 68% nitric acid and pure water in a ratio of 1:1, and the time is as long as possible.

The drying temperature in the step 7 is 100 ℃, and the time is the drying of the precipitate.

In this example, the recovery rate of ruthenium metal was 99.8%, and the recovery rate of silver metal was 99.7%.

Example 3

A precious metal recovery process based on a vacuum sputtering chamber comprises the following steps:

step 1, completely immersing a prevention plate in a nitric acid solution;

step 2, immersing the anti-sticking plate into an electrolytic solution;

step 3, immersing the anti-sticking plate into hydrofluoric acid solution;

step 4, putting the anti-sticking plate into a sand blasting machine for sand blasting treatment to finish the anti-sticking plate treatment;

step 5, filtering the solution obtained in the step 1 and the step 2 by using a filter gauze to filter out precipitate or solid ruthenium;

step 6, immersing the filtered precipitate or solid ruthenium into nitric acid solution again;

and 7, filtering the solution obtained in the step 6 by using filter gauze again, and drying to obtain the ruthenium metal.

The concentration ratio of the nitric acid solution in the step 1 is that 68 percent nitric acid and pure water are mixed in a ratio of 1:1, the soaking time is mainly that the silver layer is completely peeled off, the time is as long as possible, and the nitric acid needs to be supplemented in the middle.

And 2, adopting a mixed alkali liquor as the electrolyte in the electrolytic cell in the step 2, wherein the mixed alkali liquor is formed by mixing a sodium hydroxide solution, sodium bicarbonate and a sodium carbonate solution, and the concentration of sodium hydroxide, sodium bicarbonate and sodium carbonate in the mixed alkali liquor is 15g/L, 15g/L and 15g/L respectively. The electrolysis voltage was 60 volts and the current was 6 amps.

The concentration ratio of the hydrofluoric acid solution in the step 3 is formed by mixing experimental hydrofluoric acid and pure water in a ratio of 1:10, the soaking time is 10-20 seconds, and the reaction is carried out on the surface of the titanium plate.

The sand blasting treatment in the step 4 makes the surface roughness of the titanium plate larger, and the molybdenum sheet can be prevented from sliding when placed on the upper surface.

The filtering gauze in the step 5 is normal filtering gauze which can filter precipitated ruthenium or ruthenium hydroxide and the like in the solution.

The concentration ratio of the nitric acid solution in the step 6 is that the nitric acid solution is formed by mixing 68% nitric acid and pure water in a ratio of 1:1, and the time is as long as possible.

The drying temperature in the step 7 is 100 ℃, and the time is the drying of the precipitate.

In this example, the recovery rate of ruthenium metal was 99.7% and the recovery rate of silver metal was 99.6%.

It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.