A method for surface treatment of a backplate of a titanium target and copper backplate target assembly

Abstract

The application relates to a surface treatment method for a reverse sputtering surface in a titanium target material and a copper back plate target material assembly, in particular to the technical field of target materials, and the surface treatment method comprises the following steps: roughening treatment, chitosan treatment and plasma treatment are sequentially performed on the reverse sputtering surface; and a treatment agent used in the chitosan treatment comprises a solution containing organic acid and chitosan. The surface treatment method provided by the application can make the reverse sputtering material formed when the titanium-copper target material assembly is sputtered effectively adhere to the reverse sputtering surface of the target material through the synergistic effect of the chitosan treatment and the plasma treatment, the risk of the reverse sputtering particles falling off in the sputtering process is significantly reduced, and the uniformity of a film layer obtained through sputtering film coating is beneficially ensured.

Description

Technical Field

[0001] This invention relates to the field of target technology, and specifically to a surface treatment method for the anti-sputtering surface in a titanium target and copper backplate target assembly. Background Technology

[0002] Currently, sputtering targets are important materials used in sputtering deposition. In the sputtering machine, the target material is detached in the form of molecules, atoms or ions by being bombarded by positively charged cations 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 proceeds, the metal particles, i.e. the anti-sputtering material, 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 material, the anti-sputtering material may fall off during the sputtering process, leading to defects such as tip discharge, which is not conducive to the sputtering coating process.

[0004] To address the issue of anti-sputtering material detachment, existing technologies improve the bonding effect by roughening the anti-sputtering surface. For example, CN113846299A discloses a processing method for an anti-sputtering layer on a tantalum target. The processing method includes sequentially performing roughening treatment and melting spraying treatment on the anti-sputtering layer. This method can effectively reduce the risk of particles appearing during the sputtering process of the tantalum target and improve the service life of the target.

[0005] CN102383100A discloses a target material for preventing anti-sputtering material from peeling off and a method for forming a film layer using this target material, wherein the edge of the target material has a knurled area. This solution increases the roughness of the target material by knurling its edges, thereby increasing the adhesion of the anti-sputtering material to the target material and significantly reducing the peeling off of the anti-sputtering material.

[0006] However, the bonding strength improved by simply roughening the anti-sputtering surface is still limited, and the defect of anti-sputtering material falling off still exists. 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 titanium target and copper backing target assembly, so as to solve the defect of poor bonding between anti-sputtering particles and anti-sputtering surface in titanium target.

[0008] To achieve this objective, the present invention adopts the following technical solution:

[0009] This invention provides a surface treatment method for the anti-sputtering surface in a titanium target and copper backing target assembly, the surface treatment method comprising:

[0010] The anti-sputtering surface is subjected to roughening treatment, chitosan treatment, and plasma treatment in sequence;

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

[0012] The surface treatment method provided by this invention, by leveraging the synergistic effect of chitosan treatment and plasma treatment, enables the anti-sputtering material formed during sputtering of the titanium-copper target assembly to effectively adhere to the anti-sputtering surface of the target, significantly reducing the risk of anti-sputtering particles falling off during sputtering and helping to ensure the uniformity of the film layer obtained by sputtering.

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

[0014] As a preferred embodiment 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 embodiment of the present invention, the mass concentration of 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 embodiment of the present invention, the temperature for chitosan treatment is 30-60℃.

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

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

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

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

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

[0023] Compared with existing technical solutions, the present invention has the following beneficial effects:

[0024] The anti-sputtering surface treatment method provided by this invention uses chitosan and plasma to treat the anti-sputtering surface, which makes the anti-sputtering surface highly active under the high temperature conditions (120-150℃) of target sputtering. It can effectively combine with anti-sputtered titanium particles, significantly reduce the risk of anti-sputtered titanium particles falling off, and thus avoid the impact of anti-sputtered particle falling off on the uniformity of the coating, ensuring that the uniformity of the sputtered coating is ≥99%. Detailed Implementation

[0025] 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:

[0026] During target sputtering, anti-sputtering material is generated and adheres to a specific area of ​​the target assembly, namely the anti-sputtering zone. However, due to the high temperature of the target during sputtering, the anti-sputtering material is prone to detachment, which adversely affects the target sputtering process, such as reducing the uniformity of the sputtered film. Based on this, the present invention proposes the following solution:

[0027] This embodiment provides a surface treatment method for the anti-sputtering surface in a titanium target and copper backplate target assembly, the surface treatment method including:

[0028] The anti-sputtering surface was subjected to roughening treatment, chitosan treatment, and plasma treatment in sequence.

[0029] The titanium target material can be selected as a high-purity target material, an ultra-high-purity target material, etc.

[0030] The copper backplate includes: pure copper backplate or copper alloy backplate, such as copper-chromium alloy backplates such as C18000, C18150 or C18200, and the specific backplate can be selected as high-purity backplate, ultra-high-purity backplate, etc.

[0031] In this invention, the high purity refers to a purity of ≥99.99%.

[0032] In this invention, the ultra-high purity refers to a purity of ≥99.9999%.

[0033] The anti-splash surface refers to the area where anti-splash material accumulates. This area can be treated using existing optimized methods for anti-splash material attachment, such as forming trapezoidal grooves and / or threaded surfaces.

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

[0035] The roughening treatment can be carried out by polishing, spraying, knurling, chemical etching, etc., as long as the roughness specified in this invention is achieved.

[0036] The treatment agent used in the chitosan treatment includes a solution containing organic acids and chitosan.

[0037] In this invention, the solvent for the chitosan treatment agent can be water or other commonly used solvents in the art, and the preparation process of the treatment agent can be carried out with reference to the conventional preparation process in the art.

[0038] The organic acid includes one or a combination of at least two of formic acid, acetic acid, or propionic acid.

[0039] The organic acid in the treatment agent has a mass concentration of 2-4%, such as 2%, 2.5%, 3%, 3.5%, or 4%, but is not limited to the listed values. Other unlisted values ​​within this range are also acceptable.

[0040] The chitosan concentration 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 is not limited to the listed values. Other unlisted values ​​within this range are also acceptable.

[0041] The temperature for chitosan treatment is 30-60℃, for example, it can be 30℃, 35℃, 40℃, 45℃, 50℃, 55℃ or 60℃, but is not limited to the listed values. Other unlisted values ​​within this range are also acceptable.

[0042] The chitosan treatment time 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 is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0043] In this invention, when treating chitosan, a solution pool containing the treatment agent is formed on the roughened anti-sputtering surface by forming an open pool, or the other parts except the anti-sputtering surface are shielded, exposing only the anti-sputtering surface, and then the anti-sputtering surface is brought into contact with the silane coupling agent, or an equal amount of chitosan that has been treated with the solution pool is applied to the roughened anti-sputtering surface by brushing, spraying, or other methods.

[0044] During plasma treatment, the area outside the anti-sputtering surface can be optionally shielded to avoid affecting the performance of the target material after plasma treatment.

[0045] The working gas used in the plasma treatment includes argon.

[0046] The flow rate of the working gas used in the plasma treatment is 60-100 sccm, for example, it can be 60 sccm, 65 sccm, 70 sccm, 75 sccm, 80 sccm, 85 sccm, 90 sccm, 95 sccm or 100 sccm, but is not limited to the listed values. Other unlisted values ​​within this range are also acceptable.

[0047] The discharge power of the plasma treatment is 100-200W, for example, it can be 100W, 110W, 120W, 130W, 140W, 150W, 160W, 170W, 180W, 190W or 200W, but is not limited to the listed values. Other unlisted values ​​within this range are also acceptable.

[0048] The plasma treatment time 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., but is not limited to the listed values. Other unlisted values ​​within this range also meet the requirements.

[0049] Furthermore, to illustrate the beneficial effects of the surface treatment method for the anti-sputtering surface provided by the present invention, the following explanatory examples are provided:

[0050] In the following example, the target assembly used includes a high-purity titanium target with a purity of 99.99%, a pure copper backplate with a purity of 99.9%, and a chitosan treatment in which the area excluding the anti-sputtering surface is shielded before immersion.

[0051] Example 1

[0052] This embodiment provides a surface treatment method for the anti-sputtering surface in a titanium sputtering target assembly, as detailed below:

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

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

[0055] 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 180W, and the treatment time is 40min.

[0056] Example 2

[0057] This embodiment provides a surface treatment method for the anti-sputtering surface in a titanium sputtering target assembly, as detailed below:

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

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

[0060] 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 150W, and the treatment time is 50min.

[0061] Example 3

[0062] This embodiment provides a surface treatment method for the anti-sputtering surface in a titanium sputtering target assembly, as detailed below:

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

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

[0065] 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 200W, and the treatment time is 20min.

[0066] Example 4

[0067] This embodiment provides a surface treatment method for the anti-sputtering surface in a titanium sputtering target assembly, as detailed below:

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

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

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

[0071] Comparative Example 1

[0072] The only difference from Example 1 is that no roughening process is performed.

[0073] Comparative Example 2

[0074] The only difference from Example 1 is that chitosan treatment is not performed.

[0075] Comparative Example 3

[0076] The only difference from Example 1 is that plasma treatment is not performed.

[0077] Example 5

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

[0079] Example 6

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

[0081] Example 7

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

[0083] Example 8

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

[0085] Example 9

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

[0087] Example 10

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

[0089] Example 11

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

[0091] The target material assemblies of the above embodiments and comparative examples were subjected to magnetron sputtering. Since there is no test method in the art to detect the bonding force between the anti-sputtered material and the anti-sputtering zone, the present invention performs magnetron sputtering on the target material assemblies of the above embodiments and comparative examples under the same sputtering conditions, repeating 50 times, and observes the number of times particle problems occur to illustrate the effect of the surface treatment method of the present invention. Further evidence is obtained by detecting the uniformity of the sputtered film. The specific results are shown in Table 1 below.

[0092] Table 1

[0093]

[0094]

[0095] As shown in Table 1, the surface treatment method provided by the present invention, by taking advantage of the synergistic effect of chitosan treatment and plasma treatment, enables the anti-sputtering material formed during the sputtering of the titanium-copper target assembly to be effectively attached to the anti-sputtering surface of the target, significantly reducing the risk of anti-sputtering particles falling off during the sputtering process, and helping to ensure the uniformity of the film layer obtained by sputtering.

[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 solution of the present invention, and these simple modifications all fall within the protection scope of the present invention.

[0097] It should also be noted that the various specific technical features described in the above specific embodiments can be combined in any suitable manner without contradiction. In order to avoid unnecessary repetition, the present invention will not describe the various possible combinations separately.

[0098] Furthermore, various different embodiments of the present invention can be combined in any way, as long as they do not violate the spirit of the present invention, they should also be regarded as the content disclosed by the present invention.

Claims

1. A surface treatment method for solving the defect of poor adhesion between anti-sputtering particles and anti-sputtering surfaces in titanium sputtering targets, characterized in that, The surface treatment method includes: The anti-sputtering surface is subjected to roughening treatment, chitosan treatment, and plasma treatment in sequence; The treatment agent used in the chitosan treatment includes: a solution containing organic acids and chitosan; The organic acid in the treatment agent has a mass concentration of 2-4%; the organic acid includes one or a combination of at least two of formic acid, acetic acid, or propionic acid. The mass concentration of chitosan in the treatment agent is 2-3%; The chitosan treatment time is ≥60 min; The working gas used in the plasma treatment includes argon; the flow rate of the working gas used in the plasma treatment is 60-100 sscm. The discharge power of the plasma treatment is 100-200W; the plasma treatment time is ≥20min.

2. The surface treatment method as described in claim 1, characterized in that, The roughness Ra of the backsputtering surface after the roughening treatment is 100-300 μm.

3. The surface treatment method as described in claim 1, characterized in that, The chitosan treatment temperature is 30-60℃.

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