Method for improving adhesion of zinc sulfide ball cover conductive ring film layer

Abstract

A method for improving the adhesion of the film layer of a zinc sulfide dome conductive ring comprises the following steps: S1, roughening the part of the zinc sulfide dome conductive ring film layer to be plated; S2, wiping the roughened zinc sulfide dome clean; S3, fixing the zinc sulfide dome on a dome fixing tool to expose the roughened and cleaned part of the zinc sulfide dome; S4, heating the zinc sulfide dome to 150-180°C and then keeping the temperature constant for 10-30 min; S5, using a vacuum sputtering film plating machine to sputter and plate the inside to 1.5×10 ‑3 Pa or below, sputtering and plating, first using a nickel-chromium alloy target to sputter a first layer of nickel-chromium alloy on the roughened and cleaned part, then using a copper target to sputter a first layer of copper on the first layer of nickel-chromium alloy, alternating the nickel-chromium alloy target and the copper target to form at least two groups of conductive ring film layers with a thickness of 5-15 μm, wherein the mass ratio of chromium to nickel of the nickel-chromium alloy target is 2:8; S6, gradient cooling to a specified temperature, then taking out the dome fixing tool, and removing the zinc sulfide dome with the conductive ring film layer.

Description

Technical Field

[0001] This disclosure relates to the field of zinc sulfide shrouds, and more specifically to a method for improving the adhesion of the conductive ring film layer of a zinc sulfide shroud. Background Technology

[0002] Existing zinc sulfide spherical conductive rings are typically manufactured using two methods. One method involves attaching electrode plates to the inner wall of the spherical cover using adhesive. However, the adhesive adhesion is poor and prone to aging and detachment. The second method involves vacuum deposition of a metal film of a certain thickness onto the inner wall of the spherical cover. Typically, a metal film several hundred nanometers thick exhibits good adhesion. However, to achieve a certain resistance value, the metal film layer usually needs to be very thick, reaching several micrometers (e.g., 5 micrometers (μm) or more). Conductive rings of such thickness are very prone to detachment. Summary of the Invention

[0003] In view of the problems existing in the background art, the purpose of this disclosure is to provide a method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover, which can improve the adhesion of the conductive ring film layer of the zinc sulfide spherical cover so that the conductive ring film layer with a thickness of 5-15μm will not fall off the zinc sulfide spherical cover.

[0004] Therefore, a method for improving the adhesion of the conductive ring film layer of a zinc sulfide spherical cover includes the following steps: S1, polishing and roughening the area of ​​the zinc sulfide spherical cover to which the conductive ring film layer is plated; S2, cleaning the roughened zinc sulfide spherical cover with ultrasonic cleaning or manual wiping; S3, fixing the zinc sulfide spherical cover onto the spherical cover fixture of a vacuum sputtering coating machine, so that the spherical cover fixture exposes the roughened and cleaned area of ​​the zinc sulfide spherical cover; S4, heating the zinc sulfide spherical cover fixed in the spherical cover fixture to 150-180℃ and then holding it at that temperature for 10-30 minutes; S5, evacuating the vacuum sputtering coating machine to a vacuum level of 1.5 × 10⁻⁶. -3 Below Pa, sputtering deposition begins. First, a nickel-chromium alloy target is used to sputter a first layer of nickel-chromium alloy onto the roughened and cleaned area. Then, a copper target is used to sputter a first layer of copper onto the first layer of nickel-chromium alloy. Next, a nickel-chromium alloy target is used to sputter a second layer of nickel-chromium alloy onto the first layer of copper. Then, a copper target is used to sputter a second layer of copper onto the second layer of nickel-chromium alloy. The nickel-chromium alloy target and the copper target are sputtered alternately for at least two sets to form a conductive ring film layer with a thickness of 5-15 μm. The nickel-chromium alloy target is made of a nickel-chromium mass ratio of 2:8. S6, After the sputtering deposition in step S5 is completed, the temperature gradient of the zinc sulfide ball cover is cooled to the specified temperature. Then, the ball cover fixture is removed from the vacuum sputtering deposition machine, and the zinc sulfide ball cover with the conductive ring film layer is removed from the ball cover fixture.

[0005] The beneficial effects of this disclosure are as follows: In the method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover according to this disclosure, a conductive ring film layer with a thickness of 5-15 μm is formed by roughening in step S1, cleaning in step S2 (i.e., ultrasonic cleaning or manual wiping), fixing in step S3, heating of the zinc sulfide spherical cover in step S4, alternating sputtering of at least two sets of nickel-chromium alloy targets and copper targets in step S5, and gradient cooling in step S6. The conductive ring film layer with a thickness of 5-15 μm formed on the zinc sulfide spherical cover will not fall off from the zinc sulfide spherical cover during the tape film pulling test, thereby improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover. Attached Figure Description

[0006] Figure 1 This is a schematic diagram of a vacuum sputtering coating machine used in the method for improving the adhesion of the conductive ring film layer of zinc sulfide shroud according to the present disclosure.

[0007] Figure 2 This is a schematic diagram of step S5 in the method for improving the adhesion of the conductive ring film layer of a zinc sulfide shroud according to the present disclosure, in which nickel-chromium alloy and copper are alternately plated on the roughened and cleaned parts of the zinc sulfide shroud.

[0008] Figure 3 This is a photograph of the zinc sulfide ball cover forming the conductive ring film layer in Example 1 after the adhesion of the conductive ring film layer was tested.

[0009] Figure 4 This is a photograph of the zinc sulfide ball covering forming the conductive ring film in Comparative Example 1 after the adhesion of the conductive ring film layer was tested.

[0010] The reference numerals in the attached figures are explained as follows:

[0011] 100 Vacuum Sputtering Coating Machine

[0012] 1. Spherical cover fixing fixture

[0013] The roughened and cleaned areas of the P-zinc sulfide ball cover.

[0014] 2 Nickel-Chromium Alloy Target

[0015] 3 copper targets

[0016] 4 resistance coils Detailed Implementation

[0017] The accompanying drawings illustrate embodiments of this disclosure, and it will be understood that the disclosed embodiments are merely examples of this disclosure, which can be implemented in various forms. Therefore, the specific details disclosed herein should not be construed as limiting, but are intended only as the basis for the claims and as an illustrative basis to teach those skilled in the art how to implement this disclosure in various ways.

[0018] [Methods to improve the adhesion of the conductive ring film layer in zinc sulfide dome covers]

[0019] Reference Figure 1 and Figure 2 The method for improving the adhesion of the conductive ring film layer of the zinc sulfide dome according to this disclosure includes the following steps:

[0020] S1, Polish and roughen the part of the zinc sulfide ball cover with the conductive ring film layer;

[0021] S2, the roughened zinc sulfide ball cover is cleaned by ultrasonic cleaning or by hand wiping.

[0022] S3, fix the zinc sulfide ball cover to the ball cover fixing fixture 1 of the vacuum sputtering coating machine 100 so that the ball cover fixing fixture 1 exposes the roughened and cleaned part P of the zinc sulfide ball cover;

[0023] S4. Heat the zinc sulfide ball cover fixed in the ball cover fixture 1 to 150-180℃ and then keep it at a constant temperature for 10-30 minutes.

[0024] S5, vacuum sputtering coating machine, 100 pairs, internal vacuum leveled to 1.5×10 -3 Below Pa, sputtering deposition begins. First, a nickel-chromium alloy layer is sputtered onto the roughened and cleaned area P using a nickel-chromium alloy target 2. Then, a copper target 3 is used to sputter a first layer of copper onto the first nickel-chromium alloy layer. Next, a second layer of nickel-chromium alloy is sputtered onto the first copper layer using a nickel-chromium alloy target 2. Subsequently, a second layer of copper is sputtered onto the second nickel-chromium alloy layer using a copper target 3. The nickel-chromium alloy target 2 and the copper target 3 are sputtered alternately for at least two sets to form a conductive ring film layer with a thickness of 5-15 μm. The nickel-chromium alloy target 2 is made of a material with a chromium-nickel mass ratio of 2:8.

[0025] S6. After the sputtering coating in step S5 is completed, the temperature gradient of the zinc sulfide shroud is reduced to the specified temperature. Then, the shroud fixing fixture 1 is removed from the vacuum sputtering coating machine 100, and the zinc sulfide shroud with the conductive ring film layer is removed from the shroud fixing fixture 1.

[0026] In the method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover according to the present disclosure, a conductive ring film layer with a thickness of 5-15 μm is formed by roughening in step S1, cleaning in step S2 (i.e., ultrasonic cleaning or manual wiping), fixing in step S3, heating of the zinc sulfide spherical cover in step S4, alternating sputtering of at least two sets of nickel-chromium alloy target 2 and copper target 3 in step S5, and gradient cooling in step S6. As verified by the test process described later, the conductive ring film layer with a thickness of 5-15 μm formed on the zinc sulfide spherical cover does not fall off from the zinc sulfide spherical cover during the tape film pulling test, thereby improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover.

[0027] The roughening in step S1 and the cleaning in step S2 facilitate the bonding of the first layer of nickel-chromium alloy sputtered with the zinc sulfide shroud.

[0028] The heating of the zinc sulfide shroud in step S4 and the temperature of the plasma during vacuum sputtering in step S5 are coordinated. Compared with not heating the zinc sulfide shroud, this greatly reduces the temperature difference between the zinc sulfide shroud, the nickel-chromium alloy layer, and the copper layer. This is beneficial to the bonding between the first nickel-chromium alloy layer and the zinc sulfide shroud, as well as the bonding between the alternately sputtered nickel-chromium alloy layer and the copper layer, and the equalization of internal thermal stress.

[0029] In one example, in step S4, the zinc sulfide ball fixed in the ball fixing fixture 1 is heated to 160°C and then kept at that temperature for 20 minutes.

[0030] In one example, in step S4, the zinc sulfide ball fixed in the ball holder fixture 1 is heated using a resistance coil 4 (e.g., Figure 1 (As shown) Heating, graphite plate heating, or heating lamp heating.

[0031] In step S5, the alternating sputtering of the nickel-chromium alloy layer and the copper layer, the nickel-chromium alloy layer acts as a buffer transition, which is beneficial to the stress release between the alternating sputtered nickel-chromium alloy layer and the copper layer.

[0032] In one example, in step S5, the upper limit of the thickness of the first nickel-chromium alloy layer is the lower limit of the thickness of the first copper layer; the upper limit of the thickness of the first copper layer is the lower limit of the thickness of the second nickel-chromium alloy layer; and the upper limit of the thickness of the second nickel-chromium alloy layer is the lower limit of the thickness of the second copper layer. Thus, starting with the zinc sulfide dome, in the first two sets of sputtering, the alternating sputtering of the nickel-chromium alloy layer and the copper layer is performed such that the previous layer does not exceed the next layer, which is beneficial for stress release between the nickel-chromium alloy layer and the copper layer. Furthermore, the thickness of the nickel-chromium alloy and copper layers formed by sputtering more than two sets of nickel-chromium alloy and copper layers is the same as the thickness of the second nickel-chromium alloy layer and the second copper layer in the second set.

[0033] Specifically, in one example, in step S5, the conductive ring film layer consists of six layers: the first layer, a nickel-chromium alloy, has a thickness of 100-200 nm; the second layer, a copper layer, has a thickness of 200-1000 nm; the third layer, a nickel-chromium alloy, has a thickness of 1000-2000 nm; the fourth layer, a copper layer, has a thickness of 2000-4000 nm; the fifth layer, a nickel-chromium alloy, has a thickness of 1000-2000 nm; and the sixth layer, a copper layer, has a thickness of 2000-4000 nm. Further, in step S5, the conductive ring film layer consists of six layers: the first layer, a nickel-chromium alloy, has a thickness of 200 nm; the second layer, a copper layer, has a thickness of 1000 nm; the third layer, a nickel-chromium alloy, has a thickness of 1000 nm; the fourth layer, a copper layer, has a thickness of 3000 nm; the fifth layer, a nickel-chromium alloy, has a thickness of 1000 nm; and the sixth layer, a copper layer, has a thickness of 3000 nm.

[0034] like Figure 1 As shown, in step S5, the nickel-chromium alloy target 2 and the copper target 3 are mounted on the same rotatable arm. Both the nickel-chromium alloy target 2 and the copper target 3 can be frustum targets.

[0035] The gradient cooling in step S6 allows the stress in the conductive ring film to be released slowly.

[0036] In one example, in step S6, the temperature gradient of the zinc sulfide shroud is reduced to a specified temperature by: maintaining the temperature at a constant temperature of 20°C for 5 minutes at a time, until the temperature drops to 60°C.

[0037] The method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover may further include: step S7, after the zinc sulfide spherical cover forming the conductive ring film layer is cooled to room temperature, the adhesion of the conductive ring film layer is tested. The adhesion of the conductive ring film layer can be tested using a tape-pulling test.

[0038] [test]

[0039] Example 1

[0040] Example 1 uses the following steps:

[0041] S1, Polish and roughen the part of the zinc sulfide ball cover with the conductive ring film layer;

[0042] S2, the roughened zinc sulfide ball cover is cleaned by ultrasonic cleaning or by hand wiping.

[0043] S3, fix the zinc sulfide ball cover to the ball cover fixing fixture 1 of the vacuum sputtering coating machine 100 so that the ball cover fixing fixture 1 exposes the roughened and cleaned part P of the zinc sulfide ball cover;

[0044] S4, heat the zinc sulfide ball cover fixed in the ball cover fixture 1 to 160°C and then keep it at a constant temperature for 20 minutes;

[0045] S5, vacuum sputtering coating machine, 100 pairs, internal vacuum leveled to 1.5×10 -3At point Pa, sputtering deposition begins. First, a first layer of nickel-chromium alloy is sputtered onto the roughened and cleaned area P using a nickel-chromium alloy target 2. Then, a first layer of copper is sputtered onto the first nickel-chromium alloy layer using a copper target 3. Next, a second layer of nickel-chromium alloy is sputtered onto the first copper layer using the nickel-chromium alloy target 2, followed by another layer of copper sputtered onto the second nickel-chromium alloy layer using the copper target 3. This process is repeated three times with alternating nickel-chromium alloy target 2 and copper target 3 to form a conductive ring film with a thickness of 9.2 μm (9200 nm). The nickel-chromium alloy target 2 is made of chromium. The nickel mass ratio is 2:8. The thickness of the first nickel-chromium alloy layer is 200nm, the thickness of the second copper layer is 1000nm, the thickness of the third nickel-chromium alloy layer is 1000nm, the thickness of the fourth copper layer is 3000nm, the thickness of the fifth nickel-chromium alloy layer is 1000nm, and the thickness of the sixth copper layer is 3000nm. The nickel-chromium alloy target 2 and the copper target 3 are mounted on the same rotatable arm. The nickel-chromium alloy target 2 and the copper target 3 are sputtered alternately by the rotation of the arm. Both the nickel-chromium alloy target 2 and the copper target 3 are frustum targets.

[0046] S6. After the sputtering coating in step S5 is completed, the temperature gradient of the zinc sulfide sphere is reduced to the specified temperature. Then, the sphere fixing fixture 1 is removed from the vacuum sputtering coating machine 100, and the zinc sulfide sphere forming the conductive ring film layer is removed from the sphere fixing fixture 1. The temperature gradient of the zinc sulfide sphere is reduced to the specified temperature as follows: the temperature of the zinc sulfide sphere is reduced by 20°C for 5 minutes at a time until the temperature drops to 60°C.

[0047] Step S7: After the zinc sulfide ball cover forming the conductive ring film layer cools to room temperature, the adhesion of the conductive ring film layer is tested. The adhesion test is performed by manually applying 3M tape and pulling the 3M tape on the conductive ring film layer in the opposite direction to the adhesive end.

[0048] Comparative Example 1

[0049] Except for step S5, which does not use a sputtered nickel-chromium alloy layer (i.e., the nickel-chromium alloy target 2 and the copper target 3 do not need to be rotated alternately, but only the copper target 3 is used, and the 9200nm thick conductive ring film layer is only a single copper layer), the rest is the same as in Example 1.

[0050] Figure 3 This is a photograph of the zinc sulfide ball cover forming the conductive ring film layer in Example 1 after the adhesion of the conductive ring film layer was tested. Figure 4 This is a photograph of the zinc sulfide ball covering the conductive ring film layer in Comparative Example 1 after the adhesion test of the conductive ring film layer. From Figure 3 It can be seen that the conductive ring film layer is intact and has not peeled off. From Figure 4 It can be seen that the conductive ring film layer is incomplete and has peeled off.

[0051] Several exemplary embodiments have been described in detail above, but this document is not intended to limit itself to the explicitly disclosed combinations. Therefore, unless otherwise stated, the various features disclosed herein can be combined to form several other combinations, which are not shown for simplicity.

Claims

1. A method for improving the adhesion of the conductive ring film layer of a zinc sulfide spherical cover, characterized in that, Including the following steps: S1, Polish and roughen the part of the zinc sulfide ball cover with the conductive ring film layer; S2, the roughened zinc sulfide ball cover is cleaned by ultrasonic cleaning or by hand wiping. S3, fix the zinc sulfide ball cover to the ball cover fixing fixture (1) of the vacuum sputtering coating machine (100) so that the ball cover fixing fixture (1) exposes the roughened and cleaned part (P) of the zinc sulfide ball cover; S4, heat the zinc sulfide ball fixed in the ball fixing fixture (1) to 150-180℃ and then keep it at a constant temperature for 10-30 minutes; S5, vacuum sputtering coating machine (100) evacuates the internal vacuum to 1.5×10 -3 Below Pa, sputtering begins. First, a nickel-chromium alloy layer is sputtered onto the roughened and cleaned area (P) using a nickel-chromium alloy target (2). Then, a copper target (3) is used to sputter a first layer of copper onto the first nickel-chromium alloy layer. Next, a second layer of nickel-chromium alloy is sputtered onto the first copper layer using a nickel-chromium alloy target (2). Subsequently, a second layer of copper is sputtered onto the second nickel-chromium alloy layer using a copper target (3). The nickel-chromium alloy target (2) and the copper target (3) are used alternately for at least two sets to form a conductive ring film layer with a thickness of 5-15 μm. Among them, the nickel-chromium alloy target (2) is made of a nickel-chromium mass ratio of 2:

8. In step S5, the conductive ring film layer consists of six layers. The thickness of the first nickel-chromium alloy layer is 100-200nm; the thickness of the second copper layer is 200-1000nm; the thickness of the third nickel-chromium alloy layer is 1000-2000nm; the thickness of the fourth copper layer is 2000-4000nm; the thickness of the fifth nickel-chromium alloy layer is 1000-2000nm; and the thickness of the sixth copper layer is 2000-4000nm. S6. After the sputtering coating in step S5 is completed, the temperature gradient of the zinc sulfide sphere is reduced to the specified temperature. Then, the sphere fixing fixture (1) is taken out from the vacuum sputtering coating machine (100), and the zinc sulfide sphere forming the conductive ring film layer is removed from the sphere fixing fixture (1). In step S6, the temperature gradient of the zinc sulfide sphere is reduced to the specified temperature by: maintaining the temperature at a constant temperature of 20°C for 5 minutes until the temperature drops to 60°C.

2. The method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover according to claim 1, characterized in that, In step S4, the zinc sulfide ball cover fixed in the ball cover fixture (1) is heated to 160°C and then kept at a constant temperature for 20 minutes.

3. The method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover according to claim 1, characterized in that, In step S4, the zinc sulfide ball fixed in the ball cover fixture (1) is heated by a resistance coil (4), a graphite plate, or a heating lamp.

4. The method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover according to claim 1, characterized in that, In step S5, the conductive ring film layer consists of six layers. The thickness of the first nickel-chromium alloy layer is 200 nm; The thickness of the second copper layer is 1000nm; The thickness of the third nickel-chromium alloy layer is 1000 nm; The thickness of the fourth copper layer is 3000 nm; The fifth layer of nickel-chromium alloy is 1000 nm thick; The sixth copper layer is 3000nm thick.

5. The method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover according to claim 1, characterized in that, In step S5, the nickel-chromium alloy target (2) and the copper target (3) are mounted on the same rotatable arm; Both the nickel-chromium alloy target (2) and the copper target (3) are frustum targets.

6. The method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover according to claim 1, characterized in that, The method for improving the adhesion of the conductive ring film layer of the zinc sulfide spherical cover further includes: Step S7: After the zinc sulfide sphere covering the conductive ring film is cooled to room temperature, the adhesion of the conductive ring film is tested.

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