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

Abstract

The invention relates to a surface treatment method for an anti-sputtering surface in a titanium 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 roughening treatment, chitosan treatment and plasma treatment on the anti-sputtering surface; a treating agent used in the chitosan treatment comprises a solution containing organic acid and chitosan. According to the surface treatment method provided by the invention, by virtue of the synergistic effect of chitosan treatment and plasma treatment, the anti-sputtering object formed during sputtering of the titanium-copper target material assembly can be effectively attached to the anti-sputtering surface of the target material, so that the risk that anti-sputtering particles fall off in the sputtering process is remarkably reduced; and the uniformity of a film layer obtained by sputter coating can be 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 a titanium target and a copper backplane target assembly. Background Art

[0002] Currently, as an important material used in sputtering deposition, the target material is impacted by positively charged cations in a sputtering machine table 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., the anti-sputtering substances, gradually accumulate and increase on the anti-sputtering surface. However, due to the low bonding performance between the anti-sputtering surface and the anti-sputtering substances, the anti-sputtering substances will fall off during the sputtering process, which will further lead to defects such as tip discharge, and is not conducive to the sputtering coating process.

[0004] In view of the situation of anti-sputtering substance shedding, the prior art improves the bonding 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 performing roughening 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 substances from peeling off 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 force of the anti-sputtering substances on the target material and greatly reducing the situation of anti-sputtering substance peeling off.

[0006] However, the bonding 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 a titanium target and a copper backplane target assembly, so as to solve the defect of poor bonding force between the anti-sputtering particles and the anti-sputtering surface in the titanium target.

[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 a titanium target and a copper backplane target assembly, and the surface treatment method includes:

[0010] Performing roughening treatment, chitosan treatment and plasma treatment on the anti-sputtering surface in sequence;

[0011] The treatment agent used in the chitosan treatment includes: a solution containing an organic acid and chitosan.

[0012] The surface treatment method provided by the present invention, by means of the synergistic effect of chitosan treatment and plasma treatment, enables the back-sputtered matter formed during the sputtering of the titanium-copper target assembly to effectively adhere to the back-sputtering surface of the target, significantly reducing the risk of back-sputtered particle detachment during sputtering, and is beneficial to ensuring the uniformity of the film layer obtained by sputtering coating.

[0013] As a preferred technical solution of the present invention, the roughness Ra of the back-sputtering surface after roughening treatment is 100 - 300 μm.

[0014] As a preferred technical solution of the present invention, the organic acid includes: one or a combination of at least two of formic acid, acetic acid or propionic acid.

[0015] As a preferred technical solution of the present invention, the mass concentration of the organic acid in the treatment agent is 2 - 4%.

[0016] Preferably, the mass concentration of chitosan in the treatment agent is 2 - 3%.

[0017] As a preferred technical solution of the present invention, the temperature of the chitosan treatment is 30 - 60 °C.

[0018] As a preferred technical solution of the present invention, the time of the chitosan treatment is ≥60 min.

[0019] As a preferred technical solution of the present invention, the working gas used in the plasma treatment includes: argon.

[0020] As a preferred technical solution of the present invention, the flow rate of the working gas used in the plasma treatment is 60 - 100 sscm.

[0021] As a preferred technical solution of the present invention, the discharge power of the plasma treatment is 100 - 200 W.

[0022] As a preferred technical solution of the present invention, the time of the plasma treatment is ≥20 min.

[0023] Compared with the prior art solutions, the present invention has the following beneficial effects:

[0024] The surface treatment method for the anti-sputtering surface provided by the present invention treats the anti-sputtering surface by means of chitosan and plasma, so that the anti-sputtering surface has good activity under the high-temperature working conditions (120 - 150 °C) of target sputtering, can effectively combine with the anti-sputtering titanium particles, can significantly reduce the risk of shedding of the anti-sputtering titanium particles, and further avoids the influence of the shedding of the anti-sputtering particles on the coating uniformity, ensuring that the uniformity of the film layer obtained by sputtering coating is ≥ 99%. Detailed Embodiments

[0025] To better illustrate the present invention and facilitate understanding of its technical solutions, the typical but non-limiting embodiments of the present invention are as follows:

[0026] During the process of target sputtering, anti-sputtering substances will adhere to a specific area of the target assembly, namely the anti-sputtering area. However, since the temperature of the target is relatively high during sputtering, it is easy to cause the anti-sputtering substances to fall off, which will have an adverse impact on the target sputtering process, such as reducing the uniformity of the film layer obtained by sputtering coating. Based on this, the present invention proposes the following solutions:

[0027] This embodiment provides a surface treatment method for the anti-sputtering surface in a titanium target and a copper backplane target assembly. The surface treatment method includes:

[0028] Roughening treatment, chitosan treatment, and plasma treatment are sequentially performed on the anti-sputtering surface.

[0029] Among them, the titanium target can be selected as a high-purity target, an ultra-high-purity target, etc.

[0030] Among them, the copper backplane includes: a pure copper backplane or a copper alloy backplane, etc., such as copper chromium alloy backplanes such as C18000, C18150, or C18200. The specific backplane can be selected as a high-purity backplane, an ultra-high-purity backplane, etc.

[0031] In the present invention, the high purity means a purity ≥ 99.99%.

[0032] In the present invention, the ultra-high purity means a purity ≥ 99.9999%.

[0033] Among them, the anti-sputtering surface refers to the area where the anti-sputtering substances accumulate. This area can adopt existing methods to optimize the adhesion of the anti-sputtering substances, such as forming a trapezoidal groove, and / or a threaded surface, etc.

[0034] Among them, the roughness Ra of the anti-sputtering surface after roughening treatment is 100 - 300 μm. For example, it can be 100 μm, 120 μm, 140 μm, 160 μm, 180 μm, 200 μm, 220 μm, 240 μm, 260 μm, 280 μm, or 300 μm, etc., but not limited to the listed values. Other unlisted values within this range also meet the requirements.

[0035] Among them, the roughening treatment methods can be selected as: polishing, thermal spraying, knurling, chemical etching, etc., as long as the roughness defined in the present invention is achieved.

[0036] Among them, the treatment agent used in the chitosan treatment includes: a solution containing organic acid and chitosan.

[0037] In the present invention, the solvent of the treatment agent used in the chitosan treatment can be selected as common solvents in the art such as water, and the preparation process of the treatment agent can be carried out with reference to the conventional preparation process in the art.

[0038] Among them, the organic acid includes: one or a combination of at least two of formic acid, acetic acid or propionic acid.

[0039] Among them, the mass concentration of the organic acid in the treatment agent is 2-4%, for example, it can be 2%, 2.5%, 3%, 3.5% or 4%, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0040] Among them, the mass concentration of chitosan in the treatment agent is 2-3%, for example, it can be 2%, 2.2%, 2.4%, 2.6%, 2.8% or 3%, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0041] Among them, the temperature of the chitosan treatment is 30-60°C, for example, it can be 30°C, 35°C, 40°C, 45°C, 50°C, 55°C or 60°C, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0042] Among them, the time of the chitosan treatment is ≥60 min, for example, it can be 60 min, 65 min, 70 min, 75 min, 80 min, 85 min, 90 min, 95 min, 100 min, 105 min, 110 min, 115 min or 120 min, etc., but not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0043] In the present invention, when performing chitosan treatment, a dissolution pool for accommodating the treatment agent is formed by forming an open pool on the roughened anti-sputtering surface 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 a silane coupling agent, or an equal amount of chitosan attached after dissolution pool treatment is provided on the roughened anti-sputtering surface by means such as brushing and spraying.

[0044] Among them, when performing plasma treatment, optionally, the area other than the anti-sputtering surface can be shielded to avoid affecting the use effect of the target after plasma treatment.

[0045] Among them, the working gas used in the plasma treatment includes: argon gas.

[0046] Among them, the flow rate of the working gas used in the plasma treatment is 60 - 100 sscm. For example, it can be 60 sccm, 65 sccm, 70 sccm, 75 sccm, 80 sccm, 85 sccm, 90 sccm, 95 sccm, or 100 sccm, etc. However, it is not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0047] Among them, the discharge power of the plasma treatment is 100 - 200 W. For example, it can be 100 W, 110 W, 120 W, 130 W, 140 W, 150 W, 160 W, 170 W, 180 W, 190 W, or 200 W, etc. However, it is not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0048] Among them, the time of the plasma treatment is ≥ 20 min. For example, it can be 20 min, 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, 100 min, 110 min, or 120 min, etc. However, it is not limited to the listed values, and other unlisted values within this range also meet the requirements.

[0049] Furthermore, in order to illustrate the good effects that can be achieved by the surface treatment method for the anti-sputtering surface provided by the present invention, the following illustrative examples are used for the following description. The examples are as follows:

[0050] In the following examples, in the target assembly used, the titanium target is a high-purity titanium target with a purity of 99.99%, the backplate is a pure copper backplate with a purity of 99.9%, and in the chitosan treatment, the area except the anti-sputtering surface is shielded and then soaked.

[0051] Example 1

[0052] This example provides a surface treatment method for the anti-sputtering surface in a titanium target and a copper backplate target assembly, which is specifically as follows:

[0053] Among them, the roughness Ra of the anti-sputtering surface after the roughening treatment is 200 μm;

[0054] Among them, the treatment agent used in the chitosan treatment includes: a solution containing organic acid and chitosan. The organic acid is acetic acid, the mass concentration of the organic acid is 3%, the mass concentration of chitosan is 2%, and the solvent is water; the temperature of the chitosan treatment is 40 °C, and the time is 90 min;

[0055] Among them, the working gas used in the plasma treatment is argon, and the flow rate of the working gas is 80 sscm; the discharge power of the plasma treatment is 180 W, and the treatment time is 40 min.

[0056] Example 2

[0057] This example provides a surface treatment method for the anti-sputtering surface in a titanium target and a copper backplane target assembly, which is as follows:

[0058] Among them, the roughness Ra of the anti-sputtering surface after roughening treatment is 250 μm;

[0059] Among them, the treatment agent used in the chitosan treatment includes: a solution containing an organic acid and chitosan. The organic acid is acetic acid, the mass concentration of the organic acid is 3.5%, the mass concentration of chitosan is 2.5%, and the solvent is water; the temperature of the chitosan treatment is 50 °C, and the time is 80 min;

[0060] Among them, the working gas used in the plasma treatment is argon, and the flow rate of the working gas is 90 sscm; the discharge power of the plasma treatment is 150 W, and the treatment time is 50 min.

[0061] Example 3

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

[0063] Among them, the roughness Ra of the anti-sputtering surface after roughening treatment is 300 μm;

[0064] Among them, the treatment agent used in the chitosan treatment includes: a solution containing an organic acid and chitosan. The organic acid is propionic acid, the mass concentration of the organic acid is 4%, the mass concentration of chitosan is 3%, and the solvent is water; the temperature of the chitosan treatment is 30 °C, and the time is 90 min;

[0065] Among them, the working gas used in the plasma treatment is argon, and the flow rate of the working gas is 100 sscm; the discharge power of the plasma treatment is 200 W, and the treatment time is 20 min.

[0066] Example 4

[0067] This example provides a surface treatment method for the anti-sputtering surface in a titanium target and a copper backplane target assembly, which is as follows:

[0068] Among them, the roughness Ra of the anti-sputtering surface after roughening treatment is 100 μm;

[0069] Among them, the treatment agent used in the chitosan treatment includes: a solution containing organic acid and chitosan. The organic acid is formic acid, the mass concentration of the organic acid is 4%, the mass concentration of chitosan is 2%, and the solvent is water; the temperature of the chitosan treatment is 60 °C, and the time is 60 min;

[0070] Among them, the working gas used in the plasma treatment is argon, and the flow rate of the working gas used is 60 sscm; the discharge power of the plasma treatment is 100 W, and the treatment time is 80 min.

[0071] Comparative Example 1

[0072] The difference from Example 1 is only that the roughening treatment is not carried out.

[0073] Comparative Example 2

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

[0075] Comparative Example 3

[0076] The difference from Example 1 is only that the plasma treatment is not carried out.

[0077] Example 5

[0078] The difference from Example 1 is only that the mass concentration of the organic acid in the treatment agent used in the chitosan treatment is 1%.

[0079] Example 6

[0080] The difference from Example 1 is only that the mass concentration of chitosan in the treatment agent used in the chitosan treatment is 5%.

[0081] Example 7

[0082] The difference from Example 1 is only that the time of the chitosan treatment is 30 min.

[0083] Example 8

[0084] The difference from Example 1 is only that the working gas used in the plasma treatment includes: oxygen and argon with a volume ratio of 1:3.

[0085] Example 9

[0086] The difference from Example 1 is only that the working gas used in the plasma treatment includes: nitrogen and argon with a volume ratio of 1:3.

[0087] Example 10

[0088] The difference from Example 1 is only that the working gas used in the plasma treatment is oxygen.

[0089] Example 11

[0090] The difference from Example 1 is only that the working gas used in the plasma treatment is nitrogen.

[0091] The target assemblies processed in the above-mentioned examples and comparative examples were subjected to magnetron sputtering. Since there is no test method for detecting the binding force between the back-sputtered matter and the back-sputtering interval in the art, the present invention carried out magnetron sputtering on the target assemblies processed in the above-mentioned 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 film layer obtained by sputtering. The specific results are shown in Table 1 below.

[0092] Table 1

[0093]

[0094]

[0095] As can be seen from Table 1, for the surface treatment method provided by the present invention, by virtue of the synergistic effect of chitosan treatment and plasma treatment, the back-sputtered matter formed during the sputtering of the titanium-copper target assembly can be effectively attached to the back-sputtering surface of the target, significantly reducing the risk of shedding of back-sputtered particles during sputtering, which is beneficial to ensuring the uniformity of the film layer obtained by sputtering coating.

[0096] 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.

[0097] In addition, it should be noted that, among the various specific technical features described in the above specific embodiments, they can be combined in any suitable manner without conflict. To avoid unnecessary repetition, the present invention will not separately describe various possible combination methods.

[0098] 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 a titanium target and a copper backing plate target assembly, characterized in that: The surface treatment method comprises: The reverse sputtering surface is subjected to roughening treatment, chitosan treatment and plasma treatment in sequence; The treating agent used in the chitosan treatment includes: a solution containing organic acid and chitosan.

2. The surface treatment method according to claim 1, characterized in that: The roughness Ra of the anti-sputtering surface after the roughening treatment is 100-300 μm.

3. The surface treatment method according to claim 1, characterized in that: The organic acid includes: one or a combination of at least two of formic acid, acetic acid or propionic acid.

4. The surface treatment method according to claim 1, characterized in that: The mass concentration of the organic acid in the treatment agent is 2-4%; Preferably, the mass concentration of chitosan in the treating agent is 2-3%.

5. The surface treatment method according to claim 1, characterized in that: The temperature of the chitosan treatment is 30-60°C.

6. The surface treatment method according to claim 1, characterized in that: The chitosan treatment time is ≥60 min.

7. The surface treatment method according to claim 1, characterized in that: The working gas used in the plasma treatment includes argon gas.

8. The surface treatment method according to claim 1, characterized in that: The flow rate of the working gas used in the plasma treatment is 60-100 sscm.

9. The surface treatment method according to claim 1, characterized in that: The discharge power of the plasma treatment is 100-200W.

10. The surface treatment method according to claim 1, characterized in that: The plasma treatment time is ≥20 min.

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