A novel embedded composite target and its preparation method

Abstract

This application relates to the technical field of physical vapor deposition, specifically disclosing a novel embedded composite target and its preparation method. The preparation method of the embedded composite target disclosed in this application is as follows: the substrate material is cylindrical, with the upper and lower end faces leveled, and a circular through-hole is made at the center. The upper end face of the through-hole has a chamfer, and the inner wall of the through-hole is perpendicular to the upper and lower end faces. Threads are machined into the inner wall of the through-hole in the substrate, with a thread height of 0.1~0.3 mm and a thread pitch of 0.2~0.5 mm. The embedded material is cylindrical, with an outer diameter 0.12~0.19% larger than the inner diameter of the circular through-hole in the substrate material, and a height equal to the thickness of the substrate material. The embedded material is frozen in liquid nitrogen for 20~30 min, removed, and embedded into the circular hole in the substrate material. After standing for 5~10 min, an embedded composite target blank is obtained. Post-processing yields the final product. The preparation method of this application is simple, and the embedded composite target exhibits a tight bond and high bonding strength between the embedded material and the substrate material.

Description

Technical Field

[0001] This application relates to the technical field of physical vapor deposition, specifically to a novel embedded composite target and its preparation method. Background Technology

[0002] Physical vapor deposition (PVD) is a method that uses physical methods (such as evaporation and sputtering) to vaporize the coating material and deposit a coating on the surface of a substrate material. PVD has advantages such as low deposition temperature, fast deposition speed, simple equipment structure, and no pollution. In recent years, it has developed rapidly and is widely used in the automotive, medical, electronics, and aerospace fields. By depositing different coatings, it endows the substrate material with new functions and material properties, providing better performance and solutions for various application scenarios.

[0003] Sputtering targets play a crucial role in the coating process. They not only provide the necessary materials, but their construction and quality also affect the sputtering process and the quality of the coating. High-quality sputtering targets ensure the uniformity, density, and stability of the coating, improving its performance and lifespan. Inlaid composite sputtering targets refer to sputtering other materials onto a substrate material. By flexibly adjusting the types, proportions, and layout of the inlaid materials, specific coating structures and properties can be deposited, making it an important type of sputtering target.

[0004] Typically, inlaid composite targets use an interference fit to embed other materials. The diameter of the embedding material is generally no more than 40mm. If the diameter is too large, the embedding material may become misaligned and stuck during its downward movement. Forcing it in with a press will create gaps between the embedding material and the matrix material, resulting in poor bonding and embedding failure. Due to the small diameter of the embedding material, when preparing inlaid composite targets with a high proportion of embedding material, the only way is to increase the number of embedding materials, which complicates the preparation process. At the same time, the increased number of embedding materials also increases the interface length between the embedding material and the matrix material, correspondingly increasing the risk of gaps appearing at the interface during the use of the target. Summary of the Invention

[0005] To address the aforementioned technical problems, this application provides a novel embedded composite target material, its preparation method, and its application.

[0006] This application provides a novel method for preparing an embedded composite target, which consists of a matrix material and an embedded material, specifically including the following steps:

[0007] The base material is cylindrical in shape. The upper and lower end faces are leveled, and a circular through hole is opened in the center. The upper end face of the through hole is chamfered with a chamfer size of 0.5mm×45°~1.0mm×45°. The inner wall of the through hole is perpendicular to the upper and lower end faces.

[0008] The inner wall of the through hole in the base material is threaded, with a thread height of 0.1–0.3 mm and a thread pitch of 0.2–0.5 mm.

[0009] The inlay material is cylindrical, and the outer diameter of the cylinder of the inlay material is 0.12 to 0.19% larger than the inner diameter of the circular through hole of the base material. The height of the cylinder of the inlay material is the same as the thickness of the base material.

[0010] The embedding material is frozen in liquid nitrogen, then removed and embedded into the circular hole of the matrix material. After 5 to 10 minutes, an embedding composite target blank is obtained.

[0011] The novel inlaid composite target material is obtained after post-processing.

[0012] This application utilizes the above-mentioned technical solution, selecting a substrate material with through holes, which allows gas to escape from the bottom of the substrate material when the inlay material descends. If it were not a through hole, the gas would hinder the smooth descent of the inlay material. If the upper and lower end faces of the substrate material are not leveled, the machined through holes may be misaligned, resulting in gaps between the inlay material and the substrate material after inlay. The upper end face of the through hole has a chamfer, which allows the inlay material to descend vertically during inlay, preventing it from becoming skewed and stuck. The inner wall of the through hole in the substrate material is machined with threads, which can greatly improve the bonding strength. If the interference is too small, the bonding strength between the inlay material and the substrate material will be low; if the interference is too large, it will lead to difficulties in inlay and the inlay material may easily get stuck during its descent.

[0013] Preferably, in the base material, the thread height is 0.15-0.25 mm and the thread pitch is 0.3-0.4 mm.

[0014] In some specific implementations, the thread height in the base material can be 0.1–0.15 mm, 0.1–0.2 mm, 0.1–0.25 mm, 0.1–0.3 mm, 0.15–0.2 mm, 0.15–0.3 mm, 0.2–0.25 mm, 0.2–0.3 mm, or 0.25–0.3 mm, and the thread pitch can be 0.2–0.3 mm, 0.2–0.35 mm, 0.3–0.4 mm, 0.3–0.5 mm, 0.3–0.35 mm, 0.3–0.5 mm, 0.35–0.4 mm, 0.35–0.5 mm, or 0.4–0.5 mm.

[0015] In one specific implementation, the thread height in the base material can be 0.1mm, 0.15mm, 0.2mm, 0.25mm, or 0.3mm, and the thread pitch can be 0.2mm, 0.3mm, 0.35mm, 0.4mm, or 0.5mm.

[0016] Experimental analysis shows that selecting the above-mentioned thread specifications and dimensions in this application can further improve the bonding strength of the embedded composite target.

[0017] Preferably, the outer diameter of the cylindrical inlay material is 0.14 to 0.17% larger than the inner diameter of the circular through-hole in the base material.

[0018] In some specific embodiments, the outer diameter of the cylindrical inlay material is 0.12%, 0.14%, 0.15%, 0.16%, 0.17%, or 0.19% larger than the inner diameter of the circular through-hole in the base material.

[0019] In one specific embodiment, the outer diameter of the cylindrical inlay material is larger than the inner diameter of the circular through-hole in the base material by 0.12–0.14%, 0.12–0.15%, 0.12–0.16%, 0.12–0.17%, 0.12–0.19%, 0.14–0.15%, 0.14–0.16%, 0.14–0.19%, 0.15–0.16%, 0.15–0.17%, 0.15–0.19%, 0.16–0.17%, 0.16–0.19%, or 0.17–0.19%.

[0020] Experimental analysis shows that selecting the interference range mentioned above in this application can further improve the bonding strength of the inlaid composite target.

[0021] Preferably, the inlay material is any one of TiAl, CrAl, and Al, and the atomic percentage content of Al in the inlay material is 50-100 at.%.

[0022] Preferably, the matrix material is any one of TiSi and Ti.

[0023] In the technical solution provided in this application, the specific type of matrix material has little impact on the embedded composite target. The main thing is that the embedded material needs to contain Al, and the atomic percentage content of Al is 50-100 at.%. If the Al content is too low, the shrinkage after liquid nitrogen freezing is small, and it cannot be put into the hole after freezing, so it cannot be embedded. A lower Al content will also result in a lower bonding strength of the embedded composite target.

[0024] Preferably, the dimensions of the substrate material are: diameter of 60-200mm, thickness of 10-100mm, and through-hole wall thickness >15mm.

[0025] In the technical solution provided in this application, the size of the substrate material needs to be controlled within the above-mentioned range. If the wall thickness is too thin, the substrate material may crack after being inlaid.

[0026] Preferably, the diameter of the inlay material is 30-170 mm.

[0027] Preferably, the freezing time in liquid nitrogen is 20 to 30 minutes.

[0028] In the technical solution provided in this application, the inlay material is placed in liquid nitrogen and frozen for 20 to 30 minutes. This is mainly to ensure that the inlay material is thoroughly cooled. If the freezing time is too short, the inlay material may not shrink enough and cannot be inlaid, or it may get stuck halfway in.

[0029] Preferably, the post-processing includes the following steps:

[0030] The inlaid composite target blank is machined to remove the chamfer layer on the upper end face, and then machined to the dimensions required by the drawing by machining or grinding.

[0031] The processed inlay composite target is ultrasonically cleaned in alcohol for 5-10 minutes, and then placed in a vacuum oven and baked at 105-115℃ for 10-20 minutes.

[0032] Secondly, this application provides a novel embedded composite target material, which is prepared using the above-mentioned method for preparing novel embedded composite targets.

[0033] In summary, the technical solution of this application has the following effects:

[0034] The inlaid composite target prepared in this application has a tight bond between the inlaid material and the matrix material, and the bonding strength is high. The preparation method provided in this application can inlay large-sized inlaid materials. Compared with inlaying multiple small-sized inlaid materials, the interface length between the inlaid material and the matrix material in this application is smaller, and the risk of gaps appearing at the interface during the use of the target is lower. The process of preparing the inlaid composite target in this application is simple and can save processing costs.

[0035] This application optimizes the specifications and dimensions of the threads in the matrix material and the interference between the inlay material and the matrix material, thereby further improving the bonding strength of the inlaid composite target. Attached Figure Description

[0036] Figure 1 This is a cross-sectional schematic diagram of the composite target material embedded in this application, where 1 is the matrix material, 2 is the embedding material, and 3 is a detail view of the chamfered area.

[0037] Figure 2 This is a top view of the inlaid composite target material prepared in Example 1.

[0038] Figure 3 This is a top view of the inlaid composite target prepared for Comparative Example 1. Detailed Implementation

[0039] The present application will be further described in detail below with reference to embodiments, comparative examples and performance test results. These embodiments should not be construed as limiting the scope of protection claimed in this application.

[0040] Example

[0041] Example 1

[0042] Example 1 provides a novel inlaid composite target material.

[0043] The preparation method of the novel embedded composite target in this embodiment specifically includes the following steps:

[0044] In this embodiment, the substrate material is Ti / Si 80 / 20at%, with a diameter of 160mm, a thickness of 50mm, and a through-hole wall thickness of 25mm; the inlay material is Ti / Al 30 / 70at%.

[0045] (1) Level the upper and lower end faces of the base material, and open a circular through hole in the center. The diameter of the through hole is 110mm. The upper end face of the through hole is chamfered with a chamfer size of 0.5mm×45°. The inner wall of the through hole is perpendicular to the upper and lower end faces.

[0046] (2) Threads are machined into the inner wall of the through hole in the base material, with a thread height of 0.2 mm and a pitch of 0.3 mm;

[0047] (3) The inlay material is processed into a cylindrical shape, the outer diameter of the cylinder is 0.15% larger than the inner diameter of the circular hole of the base material (interference), and the height of the cylinder is the same as the thickness of the base material;

[0048] (4) Freeze the embedding material in liquid nitrogen for 25 minutes, take it out and embed it into the round hole of the matrix material, place it for 10 minutes, and obtain the embedding composite target blank.

[0049] (5) Remove the chamfer layer on the upper end face of the inlaid composite target blank by turning, and then continue to process it to the dimensions required by the drawing by turning or grinding.

[0050] (6) Place the processed inlay composite target in alcohol for ultrasonic cleaning for 10 minutes, and then place it in a vacuum oven and bake at 110°C for 15 minutes.

[0051] like Figure 1 The image shown is a cross-sectional schematic diagram of the inlaid composite target material of this application, where 1 is the matrix material, 2 is the inlay material, and 3 is a detail view of the chamfered area.

[0052] like Figure 2 The image shown is a top view of the inlaid composite target prepared in Example 1; the inlaid composite target has a tight bond between the inlaid material and the matrix material, and the bond strength is high.

[0053] Examples 2-5

[0054] Examples 2-5 each provide a novel inlaid composite target material.

[0055] The difference between the above embodiment and Embodiment 1 is that the thread process parameters are different, as shown below.

[0056] In Example 2: the thread height is 0.1 mm and the thread pitch is 0.3 mm.

[0057] In Example 3: the thread height is 0.3mm and the thread pitch is 0.3mm.

[0058] In Example 4: the thread height is 0.2mm and the thread pitch is 0.2mm.

[0059] In Example 5: the thread height is 0.2 mm and the thread pitch is 0.5 mm.

[0060] The above embodiments are identical to the matrix material and inlay material of the novel inlaid composite target in Embodiment 1, as well as the remaining steps of the preparation method.

[0061] Examples 6-7

[0062] Examples 6-7 each provide a novel inlaid composite target material.

[0063] The difference between the above embodiment and Embodiment 1 is that the interference process parameters are different, as shown below.

[0064] In Example 6: The interference fit process parameters are: the outer diameter of the cylindrical insert material is 0.12% larger than the inner diameter of the circular through-hole in the base material.

[0065] In Example 7: The interference fit process parameters are: the outer diameter of the cylindrical insert material is 0.19% larger than the inner diameter of the circular through-hole in the base material.

[0066] The above embodiments are identical to the matrix material and inlay material of the novel inlaid composite target in Embodiment 1, as well as the remaining steps of the preparation method.

[0067] Examples 8-10

[0068] Examples 8-10 each provide a novel inlaid composite target material.

[0069] The difference between the above embodiments and Embodiment 1 is that the inlay materials are different, as shown below.

[0070] In Example 8: the inlay material is Ti / Al 55 / 45 at%.

[0071] In Example 9: the inlay material is Ti / Al 50 / 50 at%.

[0072] In Example 10: the inlay material is Al.

[0073] The above embodiments are identical to the matrix material and inlay material of the novel inlaid composite target in Embodiment 1, as well as the remaining steps of the preparation method.

[0074] Comparative Example

[0075] Comparative Example 1

[0076] This comparative example provides a novel inlay composite target material.

[0077] The difference between this comparative example and Example 1 is that the upper and lower end faces of the substrate material are not leveled, and the inner wall of the central through hole is not perpendicular to the upper and lower end faces.

[0078] The matrix material and inlay material of this comparative example are the same as those of the novel inlaid composite target in Example 1, as well as the remaining steps of the preparation method.

[0079] like Figure 3 As shown, this is the gap between the inlay material and the matrix material of the inlaid composite target prepared in Comparative Example 1.

[0080] Comparative Example 2

[0081] This comparative example provides a novel inlay composite target material.

[0082] The difference between this comparative example and Example 1 is that no threads are machined into the inner wall of the through hole in the base material.

[0083] The matrix material and inlay material of this comparative example are the same as those of the novel inlaid composite target in Example 1, as well as the remaining steps of the preparation method.

[0084] Comparative Example 3

[0085] This comparative example provides a novel inlay composite target material.

[0086] The difference between this comparative example and Example 1 is that the inlay material is processed into a cylindrical shape, and the outer diameter of the cylinder is 0.09% larger than the inner diameter of the circular hole in the base material.

[0087] The matrix material and inlay material of this comparative example are the same as those of the novel inlaid composite target in Example 1, as well as the remaining steps of the preparation method.

[0088] Comparative Example 4

[0089] This comparative example provides a novel inlay composite target material.

[0090] The difference between this comparative example and Example 1 is that the inlay material is processed into a cylindrical shape, and the outer diameter of the cylinder is 0.22% larger than the inner diameter of the circular hole in the base material.

[0091] The matrix material and inlay material of this comparative example are the same as those of the novel inlaid composite target in Example 1, as well as the remaining steps of the preparation method.

[0092] Performance testing of bonding strength: The inlaid composite target is placed horizontally under the press head of the press. There is a pad under the inlaid composite target. The press pressure is applied to the inlaid material. When the pressure increases to a certain value P, the inlaid material will be ejected. The surface area of ​​the inner wall of the through hole of the matrix is ​​S. The bonding strength P = F / S.

[0093] Test results are shown in Table 1.

[0094] Table 1 Performance test results of the novel inlaid composite targets in Examples 1-10 and Comparative Examples 1-4

[0095]

[0096]

[0097] Based on the test results in Table 1 and using the technical solutions provided, the inlaid composite targets prepared in Examples 1-10 have a tight bond between the inlaid material and the matrix material, exhibiting high bonding strength.

[0098] In Comparative Example 1, during the preparation of the inlaid composite target, the upper and lower end faces of the substrate material were not leveled, the through holes were not aligned, and gaps existed between the inlaid material and the substrate material after inlaying. Figure 3 As shown.

[0099] In Comparative Example 2, no threads were machined into the inner wall of the through hole in the matrix material during the preparation of the inlaid composite target; in Comparative Example 3, the interference fit was too small during the preparation of the inlaid composite target, and the bonding strength of the inlaid composite target was lower than that of the embodiments of this application.

[0100] In Comparative Example 4, the interference fit was too large during the preparation of the inlaid composite target, causing the inlaid material to get stuck during its downward movement, resulting in inlay failure.

[0101] By comparing the test results of Examples 1-5, this application can further improve the bonding strength of the inlaid composite target by controlling the thread height to 0.15-0.25 mm and the thread pitch to 0.3-0.4 mm in the matrix material raw material.

[0102] By comparing the test results of Examples 1 and 6-7, this application controls the interference to be 0.15-0.18% in the matrix material raw material, that is, the outer diameter of the cylindrical inlay material is 0.15-0.18% larger than the inner diameter of the circular through hole of the matrix material, which can further improve the bonding strength of the inlay composite target.

[0103] By comparing the test results of Examples 1 and 8-10, it was found that the inlay material selected in this application needs to contain Al. If the Al content is too low, the shrinkage after liquid nitrogen freezing will be small and the bonding strength will be low. Therefore, when the atomic percentage content of Al is controlled to be 50-100 at.%, the bonding strength of the inlay composite target can be further improved.

[0104] Although the present invention has been described in detail above with general descriptions and specific embodiments, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention fall within the scope of protection claimed by the present invention.

Claims

1. A method for preparing a novel embedded composite target, characterized in that, It consists of a base material and an inlay material, and specifically includes the following steps in sequence: The base material is cylindrical in shape. The upper and lower end faces are leveled, and a circular through hole is opened in the center. The upper end face of the through hole is chamfered with a chamfer size of 0.5mm×45°~1.0mm×45°. The inner wall of the through hole is perpendicular to the upper and lower end faces. The inner wall of the through hole in the matrix material is threaded with a thread height of 0.1-0.3 mm and a pitch of 0.2-0.5 mm; the matrix material is any one of TiSi and Ti; the dimensions of the matrix material are: diameter of 60-200 mm, thickness of 10-100 mm, and through hole wall thickness >15 mm. The inlay material is cylindrical, and the outer diameter of the cylinder of the inlay material is 0.14 to 0.19% larger than the inner diameter of the circular through hole of the base material. The height of the cylinder of the inlay material is the same as the thickness of the base material. The embedding material is frozen in liquid nitrogen for 20-30 minutes, then removed and embedded into a circular hole in the substrate material. After being left for 5-10 minutes, an embedded composite target blank is obtained. The embedding material is Ti / Al30 / 70at% or Al. The diameter of the embedding material is 30-170 mm. The novel inlaid composite target material is obtained after post-processing.

2. The method for preparing the novel embedded composite target according to claim 1, characterized in that, In the base material, the thread height is 0.15–0.25 mm and the thread pitch is 0.3–0.4 mm.

3. The method for preparing the novel embedded composite target according to claim 1, characterized in that, The outer diameter of the cylindrical inlay material is 0.14 to 0.17% larger than the inner diameter of the circular through-hole in the base material.

4. The method for preparing the novel embedded composite target according to claim 1, characterized in that, The post-processing includes the following steps: The inlaid composite target blank is machined to remove the chamfer layer on the upper end face, and then machined to the dimensions required by the drawing by machining or grinding. The processed inlay composite target is ultrasonically cleaned in alcohol for 5-10 minutes, and then placed in a vacuum oven and baked at 105-115℃ for 10-20 minutes.

5. A novel inlaid composite target material, characterized in that, It is prepared using the method for preparing the novel embedded composite target as described in any one of claims 1-4.

Images