A method for enhancing the oxidation resistance of a sputter target surface

Abstract

The application relates to a treatment method for enhancing the oxidation resistance effect of a sputtering target material surface, which comprises the following steps: S1, taking the cooling surface of a back plate, the side surface of the back plate, the step surface of the back plate, the side surface of the target material and the edge area of the sputtering surface of the target material as the surfaces to be treated, performing sand blasting treatment to obtain a sand-blasted surface; and S2, performing hot melt spraying treatment on the sand-blasted surface obtained in the step S1 to complete the preparation of an oxidation-resistant coating. Through specific design of sand blasting and hot melt spraying coating, an active oxidation-resistant structure can be formed on the target material surface, and the surface oxidation resistance of the target material itself is enhanced.

Description

Technical Field

[0001] This invention relates to the field of sputtering target technology, and more specifically to a treatment method for enhancing the surface anti-oxidation effect of sputtering targets. Background Technology

[0002] Sputtering targets, especially high-purity metal and alloy targets (such as aluminum, copper, titanium, tantalum, cobalt, tungsten-titanium alloys, etc.), are core materials in advanced manufacturing fields such as semiconductor integrated circuits, flat panel displays, solar cells, and high-end optical coatings. The performance of the sputtered thin film directly determines the electrical characteristics, reliability, and lifespan of the final device, thus imposing almost stringent requirements on the purity, density, and microstructure of the target material.

[0003] However, after production, during storage and transportation, and before being loaded into the sputtering chamber, the surface of high-purity metal targets is highly susceptible to reaction with oxygen and water vapor in the air, forming an uneven oxide layer. This natural oxidation process can cause a series of serious technical problems. To avoid the effects of natural oxidation, existing processes mainly employ passive protection strategies: (1) completing the final processing and packaging in an inert atmosphere (such as Ar) glove box; (2) using vacuum bags or sealed bags filled with inert gas for packaging; and (3) applying a peelable organic protective film. However, current passive protection methods are costly, cumbersome to operate, and the packaging materials may pose a risk of contamination.

[0004] Therefore, how to proactively, effectively, and pollution-free enhance the surface oxidation resistance of high-purity sputtering targets and reduce reliance on complex external packaging and harsh storage environments is a technical problem that needs to be solved. Summary of the Invention

[0005] To address the above problems, the present invention aims to provide a treatment method that enhances the surface anti-oxidation effect of sputtering targets. Compared with the prior art, the present invention, through a specific design of sandblasting and hot melt spraying coating, can form an active anti-oxidation structure on the surface of the target, thereby enhancing the surface anti-oxidation capability of the target itself.

[0006] To achieve this objective, the present invention adopts the following technical solution: This invention provides a method for enhancing the antioxidant effect of sputtering target surface, the method comprising the following steps: S1. The cooling surface of the backplate, the side surface of the backplate, the step surface of the backplate, the side surface of the target material, and the edge area of ​​the sputtering surface of the target material in the target material assembly are used as the surfaces to be treated, and sandblasting is performed to obtain the sandblasted surface. S2, the sandblasted surface obtained in step S1 is subjected to hot melt spraying to complete the preparation of the anti-oxidation coating.

[0007] In this invention, by sandblasting specific surfaces to be treated, such as the cooling surface of the backplate, the side surface of the backplate, the stepped surface of the backplate, the side surface of the target material, and the edge area of ​​the sputtering surface of the target material, it is possible to rely on the impact of sand particles to form pits on the metal surface, thereby increasing the surface roughness of the substrate, improving the adhesion between the subsequent coating and the substrate, preventing the coating from falling off, and forming a dense anti-oxidation coating on the substrate surface through hot melt spraying, thereby enhancing the surface anti-oxidation ability of the target material itself.

[0008] Preferably, the edge region of the target sputtering surface in step S1 includes an annular region formed by extending the outer circle of the sputtering surface radially inward by ≤1 / 5R, where R represents the radius of the sputtering surface.

[0009] In this invention, the position of the annular region does not participate in sputtering. Therefore, by controlling the range of the annular region, it is possible to achieve an antioxidant effect while avoiding affecting the sputtering of the target material.

[0010] Preferably, the material of the backplate in step S1 includes copper or a copper alloy.

[0011] Preferably, the target material is made of any one or a combination of at least two of aluminum, titanium, tantalum, copper, nickel, tungsten, or silver.

[0012] Preferably, the pressure of the sandblasting treatment is 3~7MPa, for example, it can be 3MPa, 3.5MPa, 4MPa, 4.5MPa, 5MPa, 5.5MPa, 6MPa, 6.5MPa or 7MPa, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0013] In this invention, by controlling the pressure of sandblasting, the surface roughness of the substrate can be increased, thereby improving the adhesion between the subsequent coating and the backing plate and preventing the coating from peeling off.

[0014] Preferably, the sand particles used in the sandblasting process include aluminum oxide.

[0015] Preferably, the average particle size of the sand is 150~850μm, for example, it can be 150μm, 200μm, 250μm, 300μm, 350μm, 400μm, 450μm, 500μm, 550μm, 600μm, 650μm, 700μm, 750μm, 800μm or 850μm, but is not limited to the listed values, and other unlisted values ​​within the range are also applicable.

[0016] Preferably, the surface roughness Ra after sandblasting is 2~10μm, for example, it can be 2μm, 3μm, 4μm, 5μm, 6μm, 7μm, 8μm, 9μm or 10μm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0017] Preferably, the coating material used in the hot melt spraying process includes aluminum.

[0018] Preferably, when the coating material is aluminum, the purity is >99%, for example, it can be 99.1%, 99.2%, 99.3%, 99.4% or 99.5%, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0019] In this invention, the aluminum coating is specifically used to form a dense passivation film and block oxygen from penetrating into the substrate, effectively preventing oxidation.

[0020] Preferably, the spraying pressure of the hot melt spraying treatment is 10~40MPa, for example, it can be 10MPa, 12MPa, 14MPa, 16MPa, 18MPa, 20MPa, 22MPa, 24MPa, 26MPa, 28MPa, 30MPa, 32MPa, 34MPa, 36MPa, 38MPa or 40MPa, but is not limited to the listed values, and other unlisted values ​​within the range are also applicable.

[0021] In this invention, by optimally controlling the spraying pressure of the hot melt spraying process, the uniformity and density of the coating can be effectively guaranteed, thereby further improving the anti-oxidation effect.

[0022] Preferably, the hot melt temperature of the hot melt spraying treatment is 700~1000℃, for example, it can be 700℃, 750℃, 800℃, 850℃, 900℃, 950℃ or 1000℃, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0023] Preferably, the spraying speed of the hot melt spraying process is 3~15m / min, for example, it can be 3m / min, 4m / min, 5m / min, 6m / min, 7m / min, 8m / min, 9m / min, 10m / min, 11m / min, 12m / min, 13m / min, 14m / min or 15m / min, but is not limited to the listed values, and other unlisted values ​​within the range are also applicable.

[0024] Preferably, the spraying distance of the hot melt spraying treatment is 5~50cm, for example, it can be 5cm, 10cm, 15cm, 20cm, 25cm, 30cm, 35cm, 40cm, 45cm or 50cm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0025] Preferably, the thickness of the antioxidant coating is 0.2~1mm, for example, it can be 0.2mm, 0.3mm, 0.4mm, 0.5mm, 0.6mm, 0.7mm, 0.8mm, 0.9mm or 1mm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0026] As a preferred technical solution of the present invention, the processing method includes the following steps: S1, the cooling surface of the backplate, the side surface of the backplate, the stepped surface of the backplate, the side surface of the target material, and the edge area of ​​the sputtering surface of the target material are taken as the surface to be treated. The edge area of ​​the sputtering surface of the target material includes an annular area formed by extending ≤1 / 5R radially inward from the outer circle of the sputtering surface, where R represents the radius of the sputtering surface. The surface to be treated is sandblasted with alumina sand particles with an average particle size of 150~850μm under a pressure of 3~7MPa to obtain a sandblasted surface with a surface roughness Ra of 2~10μm. S2, the surface obtained in step S1 after sandblasting is subjected to hot melt spraying treatment using aluminum raw material with a purity >99% under the conditions of spraying pressure of 10~40MPa, hot melt temperature of 700~1000℃, spraying speed of 3~15m / min, and spraying distance of 5~50cm to complete the preparation of the anti-oxidation coating, the thickness of the anti-oxidation coating being 0.2~1mm.

[0027] Compared with the prior art, the present invention has the following beneficial effects: (1) The processing method provided by the present invention can form an active anti-oxidation structure on the surface of the target material without affecting the sputtering function of the target material by specifically designing the sandblasting and hot melt spraying of the surface to be treated, thereby enhancing the surface anti-oxidation ability of the target material itself. Under optimal conditions, the oxygen content reaches below 0.8wt%.

[0028] (2) The processing method provided by the present invention prepares a uniform and dense anti-oxidation coating by hot melt spraying, which can block oxygen from penetrating into the substrate and enhance the anti-oxidation effect. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of the sputtering surface of the target assembly provided in Embodiment 1 of the present invention; 1-Target material; 2-Backplate; 3-Antioxidant coating; Figure 2 This is a schematic diagram of the cooling surface of the target assembly provided in Embodiment 1 of the present invention. Detailed Implementation

[0030] The technical solution of the present invention will be further illustrated below through specific embodiments. Those skilled in the art should understand that the embodiments described are merely illustrative of the present invention and should not be construed as limiting the invention in any way.

[0031] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0032] Example 1 This embodiment provides a method for enhancing the anti-oxidation effect of sputtering target surface, such as... Figure 1 and Figure 2 As shown, the processing method includes the following steps: S1, the cooling surface of the backplate 2 (made of copper), the side surface of the backplate 2, the stepped surface of the backplate 2, the side surface of the target 1 (made of titanium), and the edge area of ​​the sputtering surface of the target 1 are the surfaces to be treated. The edge area of ​​the sputtering surface of the target 1 includes an annular area formed by extending 1 / 5R radially inward from the outer circle of the sputtering surface, where R represents the radius of the sputtering surface. The surface to be treated is sandblasted with alumina sand particles with an average particle size of 500μm under a pressure of 5MPa to obtain a sandblasted surface with a surface roughness Ra of 6μm. S2, the sandblasted surface obtained in step S1 is subjected to hot melt spraying treatment using aluminum raw material with a purity of 99.5% under the conditions of spraying pressure of 25MPa, hot melt temperature of 850℃, spraying speed of 9m / min, and spraying distance of 20cm to complete the preparation of anti-oxidation coating 3, the thickness of the anti-oxidation coating 3 being 0.6mm.

[0033] Example 2 This embodiment provides a method for enhancing the anti-oxidation effect of sputtering target surface, the method comprising the following steps: S1, the cooling surface of the backplate (made of copper), the side surface of the backplate, the stepped surface of the backplate, the side surface of the target (made of nickel), and the edge area of ​​the target sputtering surface are the surfaces to be treated. The edge area of ​​the target sputtering surface includes an annular area formed by extending 1 / 5R radially inward from the outer circle of the sputtering surface, where R represents the radius of the sputtering surface. The surface to be treated is sandblasted with alumina sand particles with an average particle size of 850μm under a pressure of 3MPa to obtain a sandblasted surface with a surface roughness Ra of 9μm. S2, the surface obtained in step S1 after sandblasting is subjected to hot melt spraying treatment using aluminum raw material with a purity of 99.5% under the conditions of spraying pressure of 10MPa, hot melt temperature of 1000℃, spraying speed of 15m / min, and spraying distance of 5cm to complete the preparation of the anti-oxidation coating, the thickness of the anti-oxidation coating being 0.3mm.

[0034] Example 3 This embodiment provides a method for enhancing the anti-oxidation effect of sputtering target surface, the method comprising the following steps: S1, the cooling surface of the backplate (made of copper), the side surface of the backplate, the stepped surface of the backplate, the side surface of the target (made of silver), and the edge area of ​​the target sputtering surface are the surfaces to be treated. The edge area of ​​the target sputtering surface includes an annular area formed by extending 1 / 5R radially inward from the outer circle of the sputtering surface, where R represents the radius of the sputtering surface. The surface to be treated is sandblasted with alumina sand particles with an average particle size of 150μm under a pressure of 7MPa to obtain a sandblasted surface with a surface roughness Ra of 3μm. S2, the surface obtained in step S1 after sandblasting is subjected to hot melt spraying treatment using aluminum raw material with a purity of 99.5% under the conditions of spraying pressure of 40MPa, hot melt temperature of 700℃, spraying speed of 3m / min and spraying distance of 50cm to complete the preparation of the anti-oxidation coating, the thickness of the anti-oxidation coating being 0.9mm.

[0035] Example 4 This embodiment provides a treatment method to enhance the anti-oxidation effect of sputtering target surface. The only difference between this treatment method and Embodiment 1 is that the sandblasting pressure is 2 MPa.

[0036] Example 5 This embodiment provides a treatment method to enhance the anti-oxidation effect of sputtering target surface. The only difference between this treatment method and Embodiment 1 is that the sandblasting pressure is 8 MPa.

[0037] Example 6 This embodiment provides a treatment method to enhance the anti-oxidation effect of sputtering target surface. The only difference between this treatment method and Embodiment 1 is that the spraying pressure of the hot melt spraying treatment is 5 MPa and the thickness of the anti-oxidation coating is 0.3 mm.

[0038] Example 7 This embodiment provides a treatment method to enhance the anti-oxidation effect of sputtering target surface. The only difference between this treatment method and Embodiment 1 is that the spraying pressure of the hot melt spraying treatment is 45 MPa and the thickness of the anti-oxidation coating is 0.7 mm.

[0039] Comparative Example 1 This comparative example provides a target assembly that differs from Example 1 only in that it does not undergo sandblasting and hot melt spraying.

[0040] The targets obtained in the above embodiments and comparative examples were tested: Oxygen content detection: The surface of the backplate in the target assembly was scanned and analyzed using a scanning electron microscope (SEM) and an energy dispersive spectroscopy (EDS) instrument to obtain the oxygen content. The results are shown in Table 1.

[0041] Table 1 As can be seen from the data in Table 1: (1) As can be seen from the data of Examples 1 to 3, the processing method provided by the present invention can achieve antioxidant protection and the oxygen content reaches below 0.8 wt%.

[0042] (2) As can be seen from the data of Examples 1 and 4-7, the present invention can further adjust the uniformity and density of the subsequent anti-oxidation coating by preferentially controlling the pressure of the sandblasting treatment, thereby further improving the anti-oxidation effect; the present invention can further adjust the thickness of the anti-oxidation coating by preferentially controlling the hot melt spraying treatment, thereby further improving the anti-oxidation effect.

[0043] (3) As can be seen from the comparison between Example 1 and Comparative Example 1, the present invention can achieve all-round protection of the target material by specifically selecting the surface to be treated, thus avoiding oxidation.

[0044] In summary, the present invention provides a sandblasting and hot melt spraying coating with a specific design that can form an active anti-oxidation structure on the surface of the target material, thereby enhancing the surface anti-oxidation ability of the target material itself.

[0045] The above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A method for enhancing the surface oxidation resistance of sputtering targets, characterized in that, The processing method includes the following steps: S1. The cooling surface of the backplate, the side surface of the backplate, the step surface of the backplate, the side surface of the target material, and the edge area of ​​the sputtering surface of the target material in the target material assembly are used as the surfaces to be treated, and sandblasting is performed to obtain the sandblasted surface. S2, the sandblasted surface obtained in step S1 is subjected to hot melt spraying to complete the preparation of the anti-oxidation coating.

2. The processing method according to claim 1, characterized in that, The edge region of the target sputtering surface in step S1 includes an annular region formed by extending the outer circle of the sputtering surface radially inward by ≤1 / 5R, where R represents the radius of the sputtering surface.

3. The processing method according to claim 1 or 2, characterized in that, The material of the backplate in step S1 includes copper or copper alloy.

4. The processing method according to any one of claims 1 to 3, characterized in that, The target material includes any one or a combination of at least two of the following: aluminum, titanium, tantalum, copper, nickel, tungsten, or silver.

5. The processing method according to any one of claims 1 to 4, characterized in that, The pressure for the sandblasting process is 3~7MPa.

6. The processing method according to any one of claims 1 to 5, characterized in that, The sandblasting process uses alumina as the abrasive particles. Preferably, the average particle size of the sand is 150~850μm.

7. The processing method according to any one of claims 1 to 6, characterized in that, The surface roughness Ra after sandblasting is 2~10μm.

8. The processing method according to any one of claims 1 to 7, characterized in that, The coating material used in the hot melt spraying process includes aluminum; Preferably, when the coating material is aluminum, its purity is >99%.

9. The processing method according to any one of claims 1 to 8, characterized in that, The spraying pressure for the hot melt spraying treatment is 10~40MPa; Preferably, the hot melt temperature of the hot melt spraying treatment is 700~1000℃; Preferably, the spraying speed of the hot melt spraying treatment is 3~15m / min; Preferably, the spraying distance for the hot melt spraying treatment is 5~50cm.

10. The processing method according to any one of claims 1 to 9, characterized in that, The thickness of the antioxidant coating is 0.2~1mm.

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