Surface treatment method for reverse sputtering surface in aluminum target and copper back plate target assembly

Abstract

The invention relates to a surface treatment method for an anti-sputtering surface in an aluminum target and copper back plate target assembly, in particular to the technical field of target materials, and the surface treatment method comprises the following steps: sequentially carrying out sand blasting treatment, silane coupling agent treatment and plasma treatment on the anti-sputtering surface; the silane coupling agent treatment comprises the step of treating the reverse sputtering surface subjected to the sand blasting treatment by adopting a silane coupling agent; the silane coupling agent is prepared from methyl triethoxy silane and gamma-methacryloxy propyl trimethoxy silane, and the mass ratio of the methyl triethoxy silane to the gamma-methacryloxy propyl trimethoxy silane is 1 to (2 to 5). According to the surface treatment method provided by the invention, the reverse sputtering surface in the target material assembly is subjected to specific treatment, so that the reverse sputtering object generated in the sputtering process can be effectively combined with the reverse sputtering surface, the reverse sputtering object is prevented from falling off, and the stability of the sputtering process is ensured.

Description

Technical Field

[0001] The present invention relates to the technical field of target materials, and particularly relates to a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly. Background Art

[0002] At present, as an important material used in sputtering deposition, the target material is impacted by positively charged cations in the sputtering machine and detached in the form of molecules, atoms or ions, and then redeposited on the target surface.

[0003] During the long-term use of the target material, metal particles will adhere and accumulate in a certain area of the target material. As sputtering progresses, the metal particles, i.e., anti-sputtering substances, gradually accumulate and increase on the anti-sputtering surface. However, due to the low binding performance between the anti-sputtering surface and the anti-sputtering substances, the anti-sputtering substances will fall off during the sputtering process, leading to defects such as tip discharge, which is not conducive to the sputtering coating process.

[0004] In response to the situation of anti-sputtering substance shedding, the prior art improves the binding effect by roughening the anti-sputtering surface. For example, CN113846299A discloses a processing method for the anti-sputtering layer of a tantalum target. The processing method includes sandblasting treatment and thermal spraying treatment on the anti-sputtering layer in sequence. This method can effectively reduce the risk of Particle during the sputtering of the tantalum target and improve the service life of the target material.

[0005] CN102383100A discloses a target material for preventing anti-sputtering substance peeling and a method for forming a film layer using this target material. The edge of the target material has a knurled area. This solution increases the roughness of the target material edge by knurling treatment, thereby increasing the adhesion of the anti-sputtering substances on the target material and greatly reducing the situation of anti-sputtering substance peeling.

[0006] However, the binding force improved only by roughening the anti-sputtering surface is still limited, and there are still defects of anti-sputtering substance shedding. Summary of the Invention

[0007] In view of the problems existing in the prior art, the purpose of the present invention is to provide a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly to solve the defect that the anti-sputtering substances fall off due to the poor binding force between the anti-sputtering substances and the anti-sputtering surface.

[0008] To achieve this purpose, the present invention adopts the following technical solutions:

[0009] The present invention provides a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly, and the surface treatment method includes:

[0010] Sequentially performing sandblasting treatment, silane coupling agent treatment, and plasma treatment on the anti-sputtering surface;

[0011] The silane coupling agent treatment includes: treating the anti-sputtering surface after sandblasting with a silane coupling agent; the silane coupling agent includes: methyltriethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:(2-5).

[0012] The surface treatment method provided by the present invention enables the anti-sputtered substances generated during the sputtering process to effectively adhere to the anti-sputtering surface through specific treatment of the anti-sputtering surface in the target assembly, thereby avoiding the shedding of anti-sputtered substances and ensuring the stability of the sputtering process.

[0013] As a preferred technical solution of the present invention, the roughness Ra of the anti-sputtering surface after sandblasting is 2-50 μm.

[0014] As a preferred technical solution of the present invention, the temperature of the silane coupling agent treatment is 25-50 °C.

[0015] As a preferred technical solution of the present invention, the time of the silane coupling agent treatment is ≥40 min.

[0016] As a preferred technical solution of the present invention, the method of plasma treatment includes: radio frequency plasma treatment.

[0017] As a preferred technical solution of the present invention, the absolute vacuum degree during the plasma treatment operation is ≤0.1 Pa.

[0018] As a preferred technical solution of the present invention, the flow rate of the working gas during the plasma treatment is 20-50 sccm.

[0019] As a preferred technical solution of the present invention, the working gas used during the plasma treatment includes: oxygen and argon with a volume ratio of 1:(2-4).

[0020] As a preferred technical solution of the present invention, the discharge power of the plasma treatment is 100-150 W.

[0021] As a preferred technical solution of the present invention, the time of the plasma treatment is ≥8 min.

[0022] Compared with the prior art solutions, the present invention has the following beneficial effects:

[0023] The surface treatment method provided by the present invention, after treating the anti-sputtering surface with a silane coupling agent, performs a one-step activation treatment with plasma, so that the anti-sputtering surface has a more excellent binding effect on aluminum particles, enabling the anti-sputtering surface to achieve efficient binding with anti-sputtering aluminum particles at the temperature state (130 - 150 °C) during the sputtering operation of the aluminum target assembly, avoiding the shedding of anti-sputtering particulate matter during the entire sputtering operation process, being beneficial to ensuring the sputtering coating effect, and ensuring that the film layer obtained by sputtering coating has good uniformity, with the film uniformity ≥ 99%. Detailed implementation manners

[0024] To better illustrate the present invention and facilitate understanding of its technical solutions, typical but non-limiting embodiments of the present invention are as follows:

[0025] During the sputtering of the target, anti-sputtering substances will adhere to a specific area of the target assembly, namely the anti-sputtering area. After sputtering for a certain period of time, due to the increase in the mass of the adherents and reaching the critical adhesion force, the anti-sputtering substances will fall off, which will have an adverse impact on the target sputtering process, such as problems like tip discharge. Based on this, the following solutions are proposed in the present invention:

[0026] This embodiment provides a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly. The surface treatment method includes:

[0027] Performing sandblasting treatment, silane coupling agent treatment, and plasma treatment on the anti-sputtering surface in sequence.

[0028] Among them, the aluminum target includes: pure aluminum target, aluminum alloy target, etc. Specifically, the target can be selected as a high-purity target, ultra-high-purity target, etc.

[0029] Among them, the copper backplane includes: pure copper backplane, copper alloy backplane, etc., such as copper-chromium alloy backplanes like C18000, C18150, or C18200. Specifically, the backplane can be selected as a high-purity backplane, ultra-high-purity backplane, etc.

[0030] In the present invention, the high purity means the purity ≥ 99.99%.

[0031] In the present invention, the ultra-high purity means the purity is above 99.9999%.

[0032] Among them, the anti-sputtering surface refers to the area where anti-sputtering substances accumulate. This area can adopt existing methods to optimize the adhesion of anti-sputtering substances, such as forming a trapezoidal groove, and / or a threaded surface, etc.

[0033] Among them, the roughness Ra of the anti-sputtering surface after sandblasting treatment is 2 - 50 μm. For example, it can be 2 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm or 50 μm, etc., but not limited to the listed values. Other unlisted values within this range also meet the requirements.

[0034] In the present invention, sandblasting treatment means using compressed air as the power to form a high-speed jet beam to spray the abrasive (copper ore sand, quartz sand, emery, iron sand, sea sand) onto the surface of the workpiece to be treated at a high speed to achieve the surface roughening effect. The control parameters in the specific sandblasting process can be reasonably selected according to the conventional technical requirements in this field, as long as the roughness requirements defined in the present invention are met.

[0035] Among them, the silane coupling agent treatment includes: treating the anti-sputtering surface after sandblasting treatment with a silane coupling agent.

[0036] In the present invention, for the silane coupling agent treatment, the corresponding anti-sputtering surface can be selected for sealing treatment to form a groove matching the anti-sputtering surface, and the silane coupling agent is placed in the groove for treatment, or other positions except the anti-sputtering surface are shielded, only the anti-sputtering surface is exposed and then the anti-sputtering surface is contacted with the silane coupling agent, so as to ensure that the silane coupling agent only acts on the anti-sputtering surface during the treatment. After the treatment is completed, it is dried and then subjected to plasma treatment.

[0037] Among them, the silane coupling agent includes: methyltriethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:(2 - 5). For example, it can be 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, 1:3, 1:3.2, 1:3.4, 1:3.6, 1:3.8, 1:4, 1:4.2, 1:4.4, 1:4.6, 1:4.8 or 1:5, etc., but not limited to the listed values. Other unlisted values within this range also meet the requirements.

[0038] Among them, the temperature of the silane coupling agent treatment is 25 - 50 °C. For example, it can be 25 °C, 30 °C, 35 °C, 40 °C, 45 °C or 50 °C, etc., but not limited to the listed values. Other unlisted values within this range also meet the requirements.

[0039] Among them, the time of the silane coupling agent treatment ≥ 40 min. For example, it can be 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, 100 min, 110 min or 120 min, etc., but not limited to the listed values. Other unlisted values within this range also meet the requirements.

[0040] Among them, when performing plasma treatment, it is optional to shield the area outside the anti-sputtering surface to avoid affecting the use effect of the target after plasma treatment.

[0041] Among them, the method of the plasma treatment includes: radio frequency plasma treatment.

[0042] Among them, the absolute vacuum degree of the operation of the plasma treatment ≤ 0.1 Pa. For example, it can be 0.1 Pa, 0.09 Pa, 0.08 Pa, 0.07 Pa, 0.06 Pa, 0.05 Pa, 0.04 Pa, 0.02 Pa, 0.01 Pa or 0.001 Pa, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0043] Among them, the flow rate of the working gas in the plasma treatment is 20 - 50 sccm. For example, it can be 20 sccm, 22 sccm, 24 sccm, 26 sccm, 28 sccm, 30 sccm, 32 sccm, 34 sccm, 36 sccm, 38 sccm, 40 sccm, 42 sccm, 44 sccm, 46 sccm, 48 sccm or 50 sccm, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0044] Among them, the working gas used in the plasma treatment includes: oxygen and argon with a volume ratio of 1:(2 - 4). For example, it can be 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, 1:3, 1:3.2, 1:3.4, 1:3.6, 1:3.8 or 1:4, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0045] Among them, the discharge power of the plasma treatment is 100 - 150 W. For example, it can be 100 W, 105 W, 110 W, 115 W, 120 W, 125 W, 130 W, 135 W, 140 W, 145 W or 150 W, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0046] Among them, the time of the plasma treatment is ≥ 8 min. For example, it can be 8 min, 9 min, 10 min, 12 min, 14 min, 16 min, 18 min, 20 min, 22 min, 24 min, 26 min, 28 min or 30 min, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0047] Further, in order to clarify the good adhesion effect of the anti-sputtering substances achieved after the surface treatment method of the anti-sputtering surface in the aluminum target and copper backplane target assembly provided by the present invention, the following practical examples are used for illustration:

[0048] In the following embodiments, for the target assembly, the purity of the aluminum target is 99.99%, the purity of the copper backplane is 99.9%, and in the silane coupling agent treatment, the area except the anti-sputtering surface is shielded and then soaked.

[0049] Example 1

[0050] This embodiment provides a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly, which is as follows:

[0051] The anti-sputtering surface is successively subjected to sandblasting treatment, silane coupling agent treatment, and plasma treatment.

[0052] Among them, the roughness Ra of the anti-sputtering surface after the sandblasting treatment is 20 μm.

[0053] Among them, the silane coupling agent treatment includes: treating the anti-sputtering surface after sandblasting treatment with a silane coupling agent; the silane coupling agent includes: methyltriethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:3; the temperature of the silane coupling agent treatment is 40 °C, and the time is 50 min;

[0054] Among them, the plasma treatment method includes: radio frequency plasma treatment; the absolute vacuum degree of the plasma treatment operation is 0.08 Pa; the flow rate of the working gas in the plasma treatment is 40 sccm; the working gas used in the plasma treatment is oxygen and argon with a volume ratio of 1:3; the discharge power of the plasma treatment is 130 W; the time of the plasma treatment is 10 min.

[0055] Example 2

[0056] This embodiment provides a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly, which is as follows:

[0057] The anti-sputtering surface is successively subjected to sandblasting treatment, silane coupling agent treatment, and plasma treatment.

[0058] Among them, the roughness Ra of the anti-sputtering surface after the sandblasting treatment is 30 μm.

[0059] Among them, the silane coupling agent treatment includes: treating the anti-sputtering surface after sandblasting treatment with a silane coupling agent; the silane coupling agent includes: methyltriethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:4; the temperature of the silane coupling agent treatment is 30 °C, and the time is 60 min;

[0060] Among them, the plasma treatment method includes: radio frequency plasma treatment; the absolute vacuum degree during the plasma treatment is 0.1 Pa; the flow rate of the working gas during the plasma treatment is 30 sccm; the working gas used in the plasma treatment is oxygen and argon with a volume ratio of 1:3; the discharge power of the plasma treatment is 120 W; the time of the plasma treatment is 8 min.

[0061] Example 3

[0062] This example provides a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly, which is as follows:

[0063] The anti-sputtering surface is successively subjected to sandblasting treatment, silane coupling agent treatment, and plasma treatment.

[0064] Among them, the roughness Ra of the anti-sputtering surface after the sandblasting treatment is 50 μm.

[0065] Among them, the silane coupling agent treatment includes: treating the anti-sputtering surface after the sandblasting treatment with a silane coupling agent; the silane coupling agent includes: methyltriethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:5; the temperature of the silane coupling agent treatment is 25 °C, and the time is 80 min;

[0066] Among them, the plasma treatment method includes: radio frequency plasma treatment; the absolute vacuum degree during the plasma treatment is 0.01 Pa; the flow rate of the working gas during the plasma treatment is 50 sccm; the working gas used in the plasma treatment is oxygen and argon with a volume ratio of 1:4; the discharge power of the plasma treatment is 100 W; the time of the plasma treatment is 25 min.

[0067] Example 4

[0068] This example provides a surface treatment method for the anti-sputtering surface in an aluminum target and a copper backplane target assembly, which is as follows:

[0069] The anti-sputtering surface is successively subjected to sandblasting treatment, silane coupling agent treatment, and plasma treatment.

[0070] Among them, the roughness Ra of the anti-sputtering surface after the sandblasting treatment is 20 μm.

[0071] Among them, the silane coupling agent treatment includes: treating the anti-sputtering surface after the sandblasting treatment with a silane coupling agent; the silane coupling agent includes: methyltriethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:2; the temperature of the silane coupling agent treatment is 50 °C, and the time is 40 min;

[0072] Among them, the plasma treatment method includes: radio frequency plasma treatment; the absolute vacuum degree of the plasma treatment operation is 0.1 Pa; the flow rate of the working gas in the plasma treatment is 20 sccm; the working gas used in the plasma treatment is oxygen and argon with a volume ratio of 1:2; the discharge power of the plasma treatment is 150 W; the time of the plasma treatment is 8 min.

[0073] Comparative Example 1

[0074] The difference from Example 1 is only that sandblasting treatment is not carried out.

[0075] Comparative Example 2

[0076] The difference from Example 1 is only that silane coupling agent treatment is not carried out.

[0077] Comparative Example 3

[0078] The difference from Example 1 is only that plasma treatment is not carried out.

[0079] Comparative Example 4

[0080] The difference from Example 1 is only that the silane coupling agent is methyltriethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 3:1.

[0081] Comparative Example 5

[0082] The difference from Example 1 is only that the silane coupling agent is vinyltrimethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:3.

[0083] Comparative Example 6

[0084] The difference from Example 1 is only that the silane coupling agent is aminopropyltrimethoxysilane and γ-methacryloxypropyltrimethoxysilane with a mass ratio of 1:3.

[0085] Comparative Example 7

[0086] The difference from Example 1 is only that the silane coupling agent is methyltriethoxysilane and vinyltrimethoxysilane with a mass ratio of 1:3.

[0087] Comparative Example 8

[0088] The difference from Example 1 is only that the silane coupling agent is methyltriethoxysilane and aminopropyltrimethoxysilane with a mass ratio of 1:3.

[0089] Example 5

[0090] The difference from Example 1 is only that the working gas used in the plasma treatment is nitrogen and argon with a volume ratio of 1:3.

[0091] Example 6

[0092] The difference from Example 1 is only that the working gas used in the plasma treatment is oxygen and argon with a volume ratio of 1:0.5.

[0093] Example 7

[0094] The difference from Example 1 is only that the working gas used in the plasma treatment is oxygen and argon with a volume ratio of 1:8.

[0095] The target assemblies processed in the above examples and comparative examples were subjected to magnetron sputtering. Since there is no test method for detecting the binding force between the back-sputtered material and the back-sputtering interval in the art, the present invention carried out magnetron sputtering on the target assemblies processed in the above examples and comparative examples under the same sputtering conditions, repeated 50 times, and observed the number of times of the Particle problem to illustrate the effect of the surface treatment method of the present invention. Further, it was corroborated by detecting the uniformity of the sputtered film layer. The specific results are shown in Table 1 below.

[0096] Table 1

[0097] Particle count Coating uniformity / % Example 1 0 99.5 Example 2 0 99.8 Example 3 0 99.7 Example 4 0 99.6 Comparative Example 1 5 95.4 Comparative Example 2 7 93.8 Comparative Example 3 6 94.4 Comparative Example 4 8 92.3 Comparative Example 5 9 91.5 Comparative Example 6 8 92.3 Comparative Example 7 5 95.1 Comparative Example 8 7 93.6 Example 5 3 97.2 Example 6 5 95.4 Example 7 4 96.6

[0098] As can be seen from Table 1, for the surface treatment method provided by the present invention, by specifically treating the back-sputtering surface in the target assembly, the back-sputtered material generated during the sputtering process can effectively bind to the back-sputtering surface, thereby avoiding the shedding of the back-sputtered material and ensuring the stability of the sputtering process.

[0099] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited to the specific details in the above embodiments. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, and these simple modifications all belong to the protection scope of the present invention.

[0100] In addition, it should be noted that, in the case of no contradiction, the various specific technical features described in the above specific embodiments can be combined in any suitable manner. In order to avoid unnecessary repetition, the present invention will not separately describe various possible combination methods.

[0101] In addition, any combination can be made between various different embodiments of the present invention, as long as it does not violate the idea of the present invention, and it should also be regarded as the content disclosed by the present invention.

Claims

1. A surface treatment method for the reverse sputtering surface in an aluminum target and a copper backing plate target assembly, characterized in that: The surface treatment method comprises: The anti-sputtering surface is sequentially subjected to sandblasting treatment, silane coupling agent treatment and plasma treatment; The silane coupling agent treatment comprises: treating the anti-sputtering surface after sandblasting with a silane coupling agent; the silane coupling agent comprises: methyltriethoxysilane and gamma-methacryloxypropyltrimethoxysilane in a mass ratio of 1:(2-5).

2. The surface treatment method according to claim 1, characterized in that: The roughness Ra of the anti-sputtering surface after the sandblasting treatment is 2-50 μm.

3. The surface treatment method according to claim 1, characterized in that: The temperature of the silane coupling agent treatment is 25-50°C.

4. The surface treatment method according to claim 1, characterized in that: The silane coupling agent treatment time is ≥40 min.

5. The surface treatment method according to claim 1, characterized in that: The plasma treatment method includes: radio frequency plasma treatment.

6. The surface treatment method according to claim 1, characterized in that: The absolute vacuum degree of the plasma treatment operation is ≤0.1Pa.

7. The surface treatment method according to claim 1, characterized in that: The flow rate of the working gas in the plasma treatment is 20-50 sccm.

8. The surface treatment method according to claim 1, characterized in that: The working gas used in the plasma treatment includes oxygen and argon in a volume ratio of 1:(2-4).

9. The surface treatment method according to claim 1, characterized in that: The discharge power of the plasma treatment is 100-150W.

10. The surface treatment method according to claim 1, characterized in that: The plasma treatment time is ≥8 min.