Molybdenum removal process on the surface of the anti-collision plate

Abstract

The present invention discloses a process for removing molybdenum from the surface of an anti-adhesion plate, comprising the following steps: providing an anti-adhesion plate with a molybdenum layer attached thereto; placing the anti-adhesion plate on a grill and pushing it into a high-temperature oven; turning on the high-temperature oven so that the temperature inside the high-temperature oven is maintained at 350°C to 600°C, and simultaneously blowing an oxidizing gas into the high-temperature oven, and fully reacting to oxidize the molybdenum layer on the anti-adhesion plate into molybdenum trioxide by the oxidizing gas; after the reaction is completed, turn off the high-temperature oven, take out the anti-adhesion plate after cooling; and perform post-treatment on the anti-adhesion plate. The process for removing molybdenum from the surface of the anti-adhesion plate of the present invention places the anti-adhesion plate with the molybdenum layer attached thereto in the oven at 350°C to 600°C for treatment, and simultaneously blows an oxidizing gas into the high-temperature oven, so that the molybdenum layer on the anti-adhesion plate is oxidized into molybdenum trioxide by the oxidizing gas, and the molybdenum trioxide will be separated from the surface of the anti-shielding plate as the oxidizing gas is blown in, thereby achieving the purpose of removing the molybdenum layer on the surface of the anti-adhesion plate.

Description

Technical Field

[0001] The present invention relates to the field of cleaning the surface of an anti-deposition plate, and more particularly to a process for removing molybdenum from the surface of an anti-deposition plate. Background Art

[0002] Physical Vapor Deposition (PVD) refers to the process of using a physical process to achieve material transfer, transferring atoms or molecules from a source to the surface of a substrate. Its function is to spray certain particles with special properties (high strength, wear resistance, heat dissipation, corrosion resistance, etc.) on a matrix with lower performance, so that the matrix has better performance. The basic methods of PVD include: vacuum evaporation, sputtering, ion plating (hollow cathode ion plating, hot cathode ion plating, arc ion plating, reactive ion plating, radio frequency ion plating, DC discharge ion plating).

[0003] During the PVD process, not only the product has a coating, but the entire chamber of the coating machine is also sputtered with a coating. To prevent the sputtered coating from contaminating the entire chamber, a removable and cleanable anti-deposition plate is usually surrounded on the inner wall of the chamber. As the PVD process progresses, the deposited coating will gradually thicken. When the coating accumulates to a certain extent, the anti-deposition plate needs to be removed for cleaning and then reused after cleaning.

[0004] For anti-deposition plates with different deposited coatings, different cleaning processes are respectively adopted. For an anti-deposition plate with a molybdenum layer (i.e., the coating is molybdenum), the traditional cleaning process is the nitric acid (30%) immersion process. By immersing molybdenum in high-concentration nitric acid, molybdenum is removed in the form of molybdic acid.

[0005] However, the reaction rate of molybdenum with nitric acid is positively correlated with the concentration of nitric acid. When the concentration of nitric acid decreases, the dissolution rate of molybdenum (the reaction rate of molybdenum with nitric acid) decreases significantly. When the concentration of nitric acid is lower than 10%, the surface of molybdenum is quickly passivated, the reaction almost stops, and molybdenum basically no longer continues to dissolve.

[0006] This results in that when using the traditional nitric acid cleaning process for an anti-deposition plate with a molybdenum layer, not only does the cleaning process take a long time, but also nitric acid needs to be replenished frequently, and the operation process is relatively cumbersome. Summary of the Invention

[0007] Based on this, it is necessary to provide a process for removing molybdenum from the surface of an anti-deposition plate that can solve the above problems.

[0008] A process for removing molybdenum from the surface of an anti-deposition plate includes the following steps:

[0009] Provide an anti-deposition plate with a molybdenum layer attached;

[0010] Place the anti-deposition plate on a grill and push it into a high-temperature oven;

[0011] Turn on the high-temperature oven so that the temperature inside the high-temperature oven is maintained at 350°C to 600°C, and at the same time, introduce an oxidizing gas into the high-temperature oven. After sufficient reaction, the molybdenum layer on the anti-adhesion plate is oxidized by the oxidizing gas into molybdenum trioxide.

[0012] After the reaction is completed, turn off the high-temperature oven, and take out the anti-adhesion plate after cooling.

[0013] Perform post-treatment on the anti-adhesion plate.

[0014] In one embodiment, the oxidizing gas is oxygen or air.

[0015] In one embodiment, in the operation of introducing an oxidizing gas into the high-temperature oven, the flow rate of the oxidizing gas is 5 L / min to 20 L / min.

[0016] In one embodiment, the operation of turning on the high-temperature oven so that the temperature inside the high-temperature oven is maintained at 350°C to 600°C is: turn on the high-temperature oven so that the temperature inside the high-temperature oven is maintained at 400°C to 500°C.

[0017] In one embodiment, in the operation of sufficient reaction to oxidize the molybdenum layer on the anti-adhesion plate into molybdenum trioxide by the oxidizing gas, the reaction time is 6 h to 8 h.

[0018] In one embodiment, the anti-adhesion plate is a titanium plate.

[0019] In one embodiment, the operation of performing post-treatment on the anti-adhesion plate is: clean the anti-adhesion plate and then dry it.

[0020] In one embodiment, after the operation of placing the anti-adhesion plate on the grill and pushing it into the high-temperature oven, before the operation of turning on the high-temperature oven, the following operation is performed: set a high-temperature filter at the air outlet of the high-temperature oven.

[0021] In one embodiment, after the operation of placing the anti-adhesion plate on the grill and pushing it into the high-temperature oven, before the operation of turning on the high-temperature oven, the following operation is performed: set a collection plate under the grill.

[0022] In one embodiment, the operation of cleaning the anti-adhesion plate and then drying it is: clean the anti-adhesion plate with nitric acid having a concentration of 20 wt% to 30 wt%, then clean it again with clean water, and finally dry it at 50°C to 200°C.

[0023] The molybdenum removal process on the surface of the anti-adhesion plate of the present invention is carried out by placing the anti-adhesion plate with a molybdenum layer attached therein in an oven at 350°C - 600°C and simultaneously blowing an oxidizing gas into the high-temperature oven, so that the molybdenum layer on the anti-adhesion plate is oxidized by the oxidizing gas into molybdenum trioxide, and the molybdenum trioxide will be separated from the surface of the anti-shielding plate as the oxidizing gas is blown in, thereby achieving the purpose of removing the molybdenum layer on the surface of the anti-adhesion plate.

[0024] Combined with specific embodiments, compared with the traditional process that only uses nitric acid, the molybdenum removal process on the surface of the anti-adhesion plate of the present invention not only greatly improves the processing speed but also has a simple process, reducing the operation process. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can be obtained based on these drawings.

[0026] Wherein:

[0027] Figure 1 is a flowchart of the molybdenum removal process on the surface of the anti-adhesion plate in an embodiment. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0028] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the drawings in the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, rather than all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.

[0029] Combined with Figure 1 , the present invention discloses a molybdenum removal process on the surface of the anti-adhesion plate in an embodiment, including the following steps:

[0030] S10. Provide an anti-adhesion plate with a molybdenum layer attached.

[0031] Generally, the anti-adhesion plate is a titanium plate.

[0032] S20. Place the anti-adhesion plate on a grill and push it into a high-temperature oven.

[0033] It should be noted that when the anti-adhesion plate is placed on the grill, stacking should be avoided.

[0034] Preferably, in this embodiment, after the operation of placing the anti-attachment plate on the grill and pushing it into the high-temperature oven, the following operations are further included: setting a high-temperature filter at the air outlet of the high-temperature oven.

[0035] Preferably, in this embodiment, after the operation of placing the anti-attachment plate on the grill and pushing it into the high-temperature oven, and before the operation of turning on the high-temperature oven, the following operations are included: setting a collection plate under the grill.

[0036] S30. Turn on the high-temperature oven so that the temperature inside the high-temperature oven is maintained at 350°C to 600°C, and at the same time, blow an oxidizing gas into the high-temperature oven, and fully react to oxidize the molybdenum layer on the anti-attachment plate into molybdenum trioxide by the oxidizing gas.

[0037] Considering that molybdenum trioxide will separate from the surface of the anti-shielding plate with the blowing of the oxidizing gas, this part of molybdenum trioxide can be collected by setting a high-temperature filter and a collection plate.

[0038] Generally speaking, the oxidizing gas is oxygen or air.

[0039] By blowing oxygen or air and maintaining the temperature inside the high-temperature oven at 350°C to 600°C, it is possible to not only oxidize the molybdenum layer on the anti-attachment plate into molybdenum trioxide, but also prevent the anti-attachment plate (titanium plate) itself from being oxidized.

[0040] Preferably, in this embodiment, in the operation of blowing the oxidizing gas into the high-temperature oven, the flow rate of the oxidizing gas is 5 L / min to 20 L / min.

[0041] Preferably, in this embodiment, the operation of turning on the high-temperature oven so that the temperature inside the high-temperature oven is maintained at 350°C to 600°C is: turning on the high-temperature oven so that the temperature inside the high-temperature oven is maintained at 400°C to 500°C.

[0042] Preferably, in this embodiment, in the operation of fully reacting to oxidize the molybdenum layer on the anti-attachment plate into molybdenum trioxide by the oxidizing gas, the reaction time is 6 h to 8 h.

[0043] S40. After the reaction is completed, turn off the high-temperature oven, and take out the anti-attachment plate after cooling.

[0044] Generally speaking, after the reaction is completed, the air blowing is also stopped accordingly. After the temperature inside the high-temperature oven drops to room temperature, the anti-attachment plate can be taken out.

[0045] S50. Perform post-treatment on the anti-attachment plate.

[0046] Preferably, in this embodiment, the operation of performing post-treatment on the anti-attachment plate is: cleaning the anti-attachment plate and then drying it.

[0047] Specifically, in this embodiment, the operation of cleaning and drying the anti-blocking plate is as follows: after cleaning the anti-blocking plate with nitric acid having a concentration of 20 wt% to 30 wt%, it is cleaned again with clean water, and finally dried at 50°C to 200°C.

[0048] The molybdenum removal process on the surface of the anti-blocking plate of the present invention is carried out by placing the anti-blocking plate with a molybdenum layer attached therein in an oven at 350°C to 600°C and simultaneously introducing an oxidizing gas into the high-temperature oven, so that the molybdenum layer on the anti-blocking plate is oxidized by the oxidizing gas into molybdenum trioxide, and the molybdenum trioxide will be separated from the surface of the anti-blocking plate along with the introduction of the oxidizing gas, thereby achieving the purpose of removing the molybdenum layer on the surface of the anti-blocking plate.

[0049] Combined with specific embodiments, compared with the traditional process that only uses nitric acid, the molybdenum removal process on the surface of the anti-blocking plate of the present invention not only greatly improves the processing speed, avoids the use of nitric acid, has a simple process, and reduces the operation process.

[0050] The following are specific embodiments. Among them, the anti-blocking plates with molybdenum layers attached are titanium plates from the same batch of a certain optoelectronic factory in Shenzhen.

[0051] Example 1

[0052] Put 20 kg of anti-blocking plates with molybdenum layers attached into a cleaning tank, place them on a grill, and push them into a high-temperature oven. At the same time, a high-temperature filter is set at the air outlet of the high-temperature oven, and a collection plate is set below the grill.

[0053] Turn on the high-temperature oven, keep the temperature in the high-temperature oven at 400°C, and simultaneously introduce air (flow rate: 10 L / min) into the high-temperature oven. React for 8 hours so that the molybdenum layer on the anti-blocking plate is oxidized into molybdenum trioxide, and it is separated from the surface of the anti-blocking plate along with the introduction of air, and finally falls on the high-temperature filter and the collection plate.

[0054] After the reaction is completed, turn off the high-temperature oven and stop blowing air at the same time. After the temperature in the high-temperature oven drops to room temperature, take out the anti-blocking plate.

[0055] Clean the anti-blocking plate with nitric acid having a concentration of 30 wt%, then clean it three times with clean water again, and finally dry it at 120°C.

[0056] Example 2

[0057] Put 20 kg of anti-blocking plates with molybdenum layers attached into a cleaning tank, place them on a grill, and push them into a high-temperature oven. At the same time, a high-temperature filter is set at the air outlet of the high-temperature oven, and a collection plate is set below the grill.

[0058] Turn on the high-temperature oven to maintain the temperature inside the high-temperature oven at 450 °C, and at the same time blow air into the high-temperature oven (flow rate: 10 L / min). React for 7 h so that the molybdenum layer on the shielding plate is oxidized to molybdenum trioxide, and it detaches from the surface of the shielding plate with the blowing of air and finally falls onto the high-temperature filter screen and the collection plate.

[0059] After the reaction is completed, turn off the high-temperature oven and stop blowing air at the same time. After the temperature inside the high-temperature oven drops to room temperature, take out the shielding plate.

[0060] Clean the shielding plate with nitric acid with a concentration of 30 wt%, then wash it with clean water three times again, and finally dry it at 120 °C.

[0061] Example 3

[0062] Put 20 kg of the shielding plate with a molybdenum layer attached into the cleaning tank, place it on the grill, and push it into the high-temperature oven. At the same time, set a high-temperature filter screen at the air outlet of the high-temperature oven and set a collection plate below the grill.

[0063] Turn on the high-temperature oven to maintain the temperature inside the high-temperature oven at 500 °C, and at the same time blow air into the high-temperature oven (flow rate: 10 L / min). React for 6 h so that the molybdenum layer on the shielding plate is oxidized to molybdenum trioxide, and it detaches from the surface of the shielding plate with the blowing of air and finally falls onto the high-temperature filter screen and the collection plate.

[0064] After the reaction is completed, turn off the high-temperature oven and stop blowing air at the same time. After the temperature inside the high-temperature oven drops to room temperature, take out the shielding plate.

[0065] Clean the shielding plate with nitric acid with a concentration of 30 wt%, then wash it with clean water three times again, and finally dry it at 120 °C.

[0066] Comparative Example 1

[0067] Prepare a cleaning solution, where the cleaning solution includes 30 wt% nitric acid.

[0068] Put 20 kg of the shielding plate with a molybdenum layer attached into the cleaning tank, and at the same time inject 5 L of the cleaning solution to immerse the shielding plate in the cleaning solution. At the same time, turn on the air agitation. After reacting for 24 h, take out the shielding plate.

[0069] After taking out the shielding plate, wash it with clean water three times and then dry it with hot air at 120 °C.

[0070] Test Example

[0071] Visually observe the states of the shielding plates after cleaning and drying in Examples 1 to 3 and Comparative Examples 1 to 3 respectively. The results are shown in Table 1 below.

[0072] Table 1

[0073]

[0074] Combined with Table 1, it can be seen that Examples 1 to 3 and Comparative Example 1 can all achieve the removal of the molybdenum layer attached to the surface of the anti-sticking plate. However, the overall time consumption of Examples 1 to 3 is significantly lower than that of Comparative Example 1.

[0075] The above-described embodiments only represent several implementation manners of the present invention. The description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the patent application. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of this invention patent shall be subject to the appended claims.

Claims

1. A molybdenum removal process for the surface of a guard plate, characterized in that, It includes the following steps: Provide a deposition plate attached with a molybdenum layer; Place the deposition plate on a grill and push it into a high-temperature oven; Turn on the high-temperature oven, maintain the temperature in the high-temperature oven at 350°C to 600°C, and simultaneously introduce an oxidizing gas into the high-temperature oven. React fully so that the molybdenum layer on the deposition plate is oxidized by the oxidizing gas to molybdenum trioxide; After the reaction is completed, turn off the high-temperature oven, cool it down, and then take out the deposition plate; Perform post-treatment on the deposition plate.

2. The molybdenum removal process on the surface of the anti-corrosion plate according to claim 1, wherein, The oxidizing gas is oxygen or air.

3. The molybdenum removal process on the surface of the anti-collision plate according to claim 2, characterized in that, In the operation of introducing the oxidizing gas into the high-temperature oven, the flow rate of the oxidizing gas is 5 L / min to 20 L / min.

4. The molybdenum removal process on the surface of the anti-collision plate according to claim 2, characterized in that, The operation of turning on the high-temperature oven to maintain the temperature in the high-temperature oven at 350°C to 600°C is: turn on the high-temperature oven to maintain the temperature in the high-temperature oven at 400°C to 500°C.

5. The molybdenum removal process on the surface of the anti-adhesion plate according to claim 4, characterized in that, In the operation of fully reacting so that the molybdenum layer on the deposition plate is oxidized by the oxidizing gas to molybdenum trioxide, the reaction time is 6 h to 8 h.

6. The molybdenum removal process on the surface of the anti-collision plate according to claim 4, wherein, The deposition plate is a titanium plate.

7. The molybdenum removal process on the surface of the anti-corrosion plate according to any one of claims 1 to 6, characterized in that, The operation of performing post-treatment on the deposition plate is: clean the deposition plate and then dry it.

8. The molybdenum removal process on the surface of the anti-collision plate according to claim 7, characterized in that, It also includes the following operation after placing the deposition plate on the grill and pushing it into the high-temperature oven and before turning on the high-temperature oven: set a high-temperature filter at the air outlet of the high-temperature oven.

9. The molybdenum removal process on the surface of the anti-adhesion plate according to claim 8, characterized in that, It also includes the following operation after placing the deposition plate on the grill and pushing it into the high-temperature oven and before turning on the high-temperature oven: set a collection plate under the grill.

10. The molybdenum removal process on the surface of the anti-corrosion plate according to claim 7, characterized in that, The operation of cleaning the deposition plate and then drying it is: clean the deposition plate with nitric acid with a concentration of 20 wt% to 30 wt%, then clean it again with clean water, and finally dry it at 50°C to 200°C.

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