Amorphous thin film, method for preparing the same, and use thereof
By preparing AlSiC amorphous thin films, the problem of insufficient toughness of amorphous thin films was solved, achieving a combination of high strength, high hardness and high toughness, and extending service life.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2026-03-17
AI Technical Summary
In practical applications, amorphous thin films are prone to brittle fracture due to insufficient toughness, which shortens their service life.
AlSiC amorphous thin films composed of Al, Si, and C were prepared by magnetron sputtering, with controlled atomic ratios of 20.6%-22.8% Al, 33.1%-34.7% Si, and 42.5%-46.3% C, and thicknesses of 800 nm-2 μm, forming disordered thin films.
This technology integrates high strength, high hardness, and high toughness in amorphous thin films, enhancing their protective effect and extending their service life.
Smart Images
Figure CN119465026B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of materials technology, and in particular to an amorphous thin film, its preparation method, and its application. Background Technology
[0002] Amorphous thin films are composed of randomly arranged atoms. This disorder leads to a long-range disorder and short-range order in their internal bonding structure, which gives amorphous thin films high hardness and strength, but also low toughness. In practical applications, when amorphous thin films are subjected to loads, they are prone to brittle fracture due to insufficient toughness, thus shortening their service life. Summary of the Invention
[0003] Therefore, it is necessary to provide an amorphous thin film, its preparation method and application, which has high strength, high hardness and high toughness, and has a longer service life when used as a surface protection material.
[0004] An amorphous thin film, wherein the amorphous thin film is an AlSiC amorphous thin film, composed of Al, Si and C.
[0005] In one embodiment, the amorphous thin film is composed of 20.6%-22.8% Al, 33.1%-34.7% Si and 42.5%-46.3% C by atomic fraction.
[0006] In one embodiment, the thickness of the amorphous thin film is 800 nm to 2 μm.
[0007] A method for preparing the aforementioned amorphous thin film includes the following steps:
[0008] Provide target materials;
[0009] The amorphous thin film was deposited on the substrate using magnetron sputtering.
[0010] In one embodiment, the target material is selected from a composite material of Al and SiC.
[0011] In one embodiment, the mass ratio of Al to SiC in the Al and SiC composite material is 3:7.
[0012] In one embodiment, during the magnetron sputtering step, the applied radio frequency power during deposition is 500W-600W.
[0013] In one embodiment, during the magnetron sputtering step, the deposition gas pressure is 0.32 Pa to 0.36 Pa.
[0014] In one embodiment, the deposition time in the magnetron sputtering step is 7200 seconds to 18000 seconds.
[0015] One of the aforementioned amorphous thin films is used as a surface protection material.
[0016] This invention employs a disordered arrangement of Al, Si, and C atoms to form an AlSiC amorphous thin film, which enables the AlSiC amorphous thin film to possess high strength, high hardness, and high toughness, thus achieving a strong and tough integrated structure. Consequently, when the AlSiC amorphous thin film of this invention is used as a surface protection material, it provides excellent protection and has a longer service life.
[0017] Meanwhile, this invention uses magnetron sputtering to prepare AlSiC amorphous thin films, which has a stable deposition rate. The deposited AlSiC amorphous thin films have uniform composition, dense structure, few defects, and good adhesion to the substrate. Therefore, when the AlSiC amorphous thin film of this invention is used as a surface protection material and formed on the surface of the part to be protected by magnetron sputtering, the AlSiC amorphous thin film has a good bonding effect with the part to be protected, is not easy to peel off, and has high strength, high hardness and high toughness, resulting in good protective effect and long service life. Attached Figure Description
[0018] To more clearly illustrate the technical solutions in the embodiments of this application or the conventional technology, the drawings used in the description of the embodiments or the conventional technology will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0019] Figure 1 The image shows the AFM surface morphology of the AlSiC amorphous thin film prepared in Example 1 of this invention.
[0020] Figure 2 This is a low-magnification TEM image of the AlSiC amorphous thin film prepared in Example 2 of the present invention;
[0021] Figure 3 The images show the TEM selected area electron diffraction pattern and high-resolution image of the AlSiC amorphous thin film prepared in Example 2 of this invention, where a is the TEM selected area electron diffraction pattern and b is the high-resolution image.
[0022] Figure 4 The loading-unloading curves are shown in the nanoindentation of the AlSiC amorphous thin film prepared in Example 2 of this invention.
[0023] Figure 5 This is a surface morphology image of the AlSiC amorphous thin film prepared in Example 2 of the present invention after nano-scratching. Detailed Implementation
[0024] To facilitate understanding of the present invention, it will be described in more detail below. However, it should be understood that the present invention can be implemented in many different forms and is not limited to the embodiments or examples described herein. Rather, these embodiments or examples are provided to make the disclosure of the present invention more thorough and complete.
[0025] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the specification of this invention is for the purpose of describing particular embodiments or examples only and is not intended to limit the invention. The optional scope of the term "and / or" as used herein includes any one of two or more of the related listed items, as well as any and all combinations of the related listed items, including any two related listed items, any more related listed items, or a combination of all related listed items.
[0026] In this invention, numerical ranges are involved. Unless otherwise specified, the numerical ranges are considered continuous and include the minimum and maximum values of the range, as well as every value between the minimum and maximum values. Furthermore, when the range refers to integers, it includes every integer between the minimum and maximum values of the range. Additionally, when multiple ranges are provided to describe features or characteristics, the ranges may be merged. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges to which they are included.
[0027] The amorphous thin film provided by this invention is an AlSiC amorphous thin film, composed of Al, Si, and C. It can be understood that the Al, Si, and C atoms in the AlSiC amorphous thin film are arranged in a disordered manner. Through the selection of the components of the amorphous thin film, this invention enables the amorphous thin film to possess high strength, high hardness, and high toughness, achieving a combination of strength and toughness. Furthermore, when the AlSiC amorphous thin film of this invention is used as a surface protective material, it provides excellent protection and has a longer service life.
[0028] Preferably, the amorphous thin film, by atomic fraction, is composed of 20.6%-22.8% Al, 33.1%-34.7% Si, and 42.5%-46.3% C. For example, the amorphous thin film is composed of 20.6% Al, 33.1% Si, and 46.3% C; or, the amorphous thin film is composed of 21.0% Al, 33.5% Si, and 45.5% C; or, the amorphous thin film... The thin film is composed of 21.5% Al, 34.0% Si and 44.5% C, or the amorphous thin film is composed of 22.0% Al, 34.5% Si and 43.5% C, or the amorphous thin film is composed of 22.8% Al, 34.7% Si and 42.5% C. With this configuration, the amorphous thin film can better balance toughness while having high strength and high hardness, achieving a combination of strength and toughness.
[0029] Preferably, the thickness of the amorphous thin film is 800 nm to 2 μm, for example, 800 nm, 900 nm, 1 μm, 1.1 μm, 1.2 μm, 1.3 μm, 1.4 μm, 1.5 μm, 1.6 μm, 1.7 μm, 1.8 μm, 1.9 μm, 2 μm, or any combination of these values.
[0030] The main methods for preparing amorphous thin films include physical vapor deposition, liquid phase quenching, and reaction methods. Among these, magnetron sputtering offers a stable deposition rate, resulting in amorphous thin films with uniform composition, dense structure, few defects, good adhesion to the substrate, and strong bonding. Therefore, this invention also provides a method for preparing the amorphous thin film using magnetron sputtering, comprising the following steps:
[0031] Provide target materials;
[0032] The amorphous thin film was deposited on the substrate using magnetron sputtering.
[0033] Different target materials result in different effects on the deposited amorphous thin films. In this invention, the target material is preferably a composite material of Al and SiC. Furthermore, by controlling the mass ratio of Al to SiC in the target material, the atomic ratio of Al, Si, and C in the obtained AlSiC amorphous thin film can be adjusted. Preferably, the mass ratio of Al to SiC in the Al and SiC composite material is 3:7. Therefore, combined with the deposition process conditions, an AlSiC amorphous thin film composed of 20.6%-22.8% Al, 33.1%-34.7% Si, and 42.5%-46.3% C can be obtained.
[0034] In the magnetron sputtering process, certain process conditions can affect the density and energy of the deposited particles, thereby affecting the deposition rate and the microstructure of the film. Preferably, the radio frequency power applied during deposition in this invention is 500W-600W, such as 500W, 550W, 600W, or any combination of these values, and the deposition pressure is 0.32Pa-0.36Pa, such as 0.32Pa, 0.33Pa, 0.34Pa, 0.35Pa, 0.36Pa, or any combination of these values, to obtain amorphous films of better quality.
[0035] Furthermore, in the magnetron sputtering step, the deposition time is preferably 7200 seconds to 18000 seconds, thereby obtaining an amorphous thin film of the required thickness by controlling the deposition time.
[0036] It is understood that the magnetron sputtering method of the present invention does not limit the substrate, which can be a silicon substrate or other metal substrate. Before depositing the amorphous thin film, it is preferable to perform vacuum etching on the substrate and sputter cleaning on the target to remove contaminants on the surface of the substrate and the target.
[0037] Since the amorphous film of the present invention has high strength, high hardness and high toughness, the present invention also uses the amorphous film as a surface protection material, which can not only provide better protection, but also have a longer service life.
[0038] It is understood that when the amorphous thin film of the present invention is used as a surface protection material, the part to be protected can be directly used as a substrate for magnetron sputtering, so that the AlSiC amorphous thin film is directly formed on the surface of the part to be protected. In this way, not only does the AlSiC amorphous thin film have a good bonding effect with the part to be protected and is not easy to peel off, but the AlSiC amorphous thin film also has high strength, high hardness and high toughness, good protection effect and long service life.
[0039] The following specific embodiments will further illustrate the amorphous thin film, its preparation method, and its applications.
[0040] Example 1
[0041] A single-crystal silicon substrate is fixed onto a base plate, and an automated sample feeding device delivers the base plate into a magnetron sputtering deposition chamber. A vacuum is then evacuated to a vacuum level of 5 × 10⁻⁶. -4 Argon gas was introduced into the vacuum chamber at a flow rate of 110 sccm. The etching was first performed at a power of 200 W for 30 s, followed by etching at a power of 300 W for 200 s.
[0042] A composite material of Al and SiC (Al: 30 wt.%, SiC: 70 wt.%) was provided as the target material. The surface of the target material was cleaned using an RF power supply at 200 W for 30 seconds.
[0043] Then, an AlSiC amorphous thin film was deposited on a single-crystal silicon substrate using magnetron sputtering. During the magnetron sputtering step, an RF power supply of 600W was used, the deposition gas pressure was 0.34Pa, the substrate rotation speed was 10 r / min, and the deposition time was 7200 seconds. After the deposition process, an automatic sampling device removed the substrate from the vacuum chamber, yielding an AlSiC amorphous thin film with a thickness of 800 nm. The Al amorphous thin film contained 22.0% Al, 34.5% Si, and 43.5% C atoms.
[0044] like Figure 1 The image shown is an AFM surface morphology image of the AlSiC amorphous thin film prepared in this embodiment. Figure 1 It can be seen that the surface of the AlSiC amorphous film is smooth with a roughness of 0.9 nm.
[0045] In addition, after testing, the AlSiC amorphous film prepared in this embodiment has a hardness of 16.64 GPa, a Young's modulus of 192.18 GPa, and no cracks appear when the nano-scratch load reaches 100 mN.
[0046] Example 2
[0047] A single-crystal silicon substrate is fixed onto a base plate, and an automated sample feeding device delivers the base plate into a magnetron sputtering deposition chamber. A vacuum is then evacuated to a vacuum level of 5 × 10⁻⁶. -4 Argon gas was introduced into the vacuum chamber at a flow rate of 110 sccm. The etching was first performed at a power of 200 W for 30 s, followed by etching at a power of 300 W for 200 s.
[0048] A composite material of Al and SiC (Al: 30 wt.%, SiC: 70 wt.%) was provided as the target material. The surface of the target material was cleaned using an RF power supply at 200 W for 30 seconds.
[0049] Then, an AlSiC amorphous thin film was deposited on a single-crystal silicon substrate using magnetron sputtering. During the magnetron sputtering step, an RF power supply of 600W was used, the deposition gas pressure was 0.34Pa, the substrate rotation speed was 10 r / min, and the deposition time was 18000 seconds. After the deposition process, an automatic sampling device removed the substrate from the vacuum chamber, yielding an AlSiC amorphous thin film with a thickness of 2 μm. The Al amorphous thin film contained 20.6% Al, 33.1% Si, and 46.3% C atoms.
[0050] In this embodiment, a Pt protective layer was formed on the surface of the AlSiC amorphous thin film, and then TEM testing was performed. Figure 2This is a low-magnification TEM image, showing, from top to bottom, a Pt protective layer, an AlSiC amorphous thin film, and a Si substrate. Figure 2 It can be seen that AlSiC amorphous thin films have a uniform structure, dense structure, and few defects; Figure 3 For TEM selected area electron diffraction patterns and high-resolution images, by Figure 3 It can be seen that the atomic arrangement of the Si matrix is very regular and highly ordered. In contrast, in the AlSiC amorphous film on the surface of the Si matrix, the Al, Si and C atoms do not exhibit the regular atomic arrangement of the Si matrix. Their atomic arrangement is disordered, presenting a completely disordered amorphous structure.
[0051] Figure 4 The loading-unloading curves in the nanoindentation of the AlSiC amorphous thin film prepared in this embodiment are shown below. Figure 4 It can be seen that the AlSiC amorphous thin film prepared in this embodiment has a hardness of 17.37 GPa and a Young's modulus of 193.39 GPa.
[0052] Figure 5 The image shows the surface morphology of the AlSiC amorphous thin film after nano-scratching prepared in this embodiment. The load was gradually increased from 0 to 100 mN. Figure 5 It can be seen that no cracks or failures occurred even when the nano-scratching load reached 100mN, indicating that the AlSiC amorphous film has good toughness and high bonding strength with the substrate.
[0053] Example 3
[0054] A single-crystal silicon substrate is fixed onto a base plate, and an automated sample feeding device delivers the base plate into a magnetron sputtering deposition chamber. A vacuum is then evacuated to a vacuum level of 5 × 10⁻⁶. -4 Argon gas was introduced into the vacuum chamber at a flow rate of 110 sccm. The etching was first performed at a power of 200 W for 30 s, followed by etching at a power of 300 W for 200 s.
[0055] A composite material of Al and SiC (Al: 30 wt.%, SiC: 70 wt.%) was provided as the target material. The surface of the target material was cleaned using an RF power supply at 200 W for 30 seconds.
[0056] Then, an AlSiC amorphous thin film was deposited on a single-crystal silicon substrate using magnetron sputtering. During the magnetron sputtering step, an RF power supply of 500W was used, the deposition gas pressure was 0.32 Pa, the substrate rotation speed was 10 r / min, and the deposition time was 18000 seconds. After the deposition process, an automatic sampling device removed the substrate from the vacuum chamber, yielding an AlSiC amorphous thin film with a thickness of 1.8 μm. The Al amorphous thin film contained 22.8% Al, 34.7% Si, and 42.5% C atoms.
[0057] After testing, the AlSiC amorphous film prepared in this embodiment has a hardness of 16.56 GPa, a Young's modulus of 191.09 GPa, and no cracks appear when the nano-scratching load reaches 100 mN.
[0058] Example 4
[0059] A single-crystal silicon substrate is fixed onto a base plate, and an automated sample feeding device delivers the base plate into a magnetron sputtering deposition chamber. A vacuum is then evacuated to a vacuum level of 5 × 10⁻⁶. -4 Argon gas was introduced into the vacuum chamber at a flow rate of 110 sccm. The etching was first performed at a power of 200 W for 30 s, followed by etching at a power of 300 W for 200 s.
[0060] A composite material of Al and SiC (Al: 30 wt.%, SiC: 70 wt.%) was provided as the target material. The surface of the target material was cleaned using an RF power supply at 200 W for 30 seconds.
[0061] Then, an AlSiC amorphous thin film was deposited on a single-crystal silicon substrate using magnetron sputtering. During the magnetron sputtering step, an RF power supply of 550W was used, the deposition gas pressure was 0.33Pa, the substrate rotation speed was 10 r / min, and the deposition time was 18000 seconds. After the deposition process, an automatic sampling device removed the substrate from the vacuum chamber, yielding an AlSiC amorphous thin film with a thickness of 1.9 μm. The Al amorphous thin film contained 21.0% Al, 33.5% Si, and 45.5% C atoms.
[0062] After testing, the AlSiC amorphous film prepared in this embodiment has a hardness of 16.94 GPa, a Young's modulus of 192.21 GPa, and no cracks appear when the nano-scratching load reaches 100 mN.
[0063] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0064] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.
Claims
1. An amorphous thin film, characterized by, The amorphous thin film is an AlSiC amorphous thin film composed of Al, Si and C, the three atoms of Al, Si and C in the AlSiC amorphous thin film are arranged in disorder, and the amorphous thin film is composed of 20.6%-22.8% of Al, 33.1%-34.7% of Si and 42.5%-46.3% of C in terms of atomic fraction.
2. The amorphous thin film according to claim 1, wherein The thickness of the amorphous thin film is 800 nm-2 μm.
3. A method for producing an amorphous thin film as claimed in any one of claims 1-2, characterized in that, The method comprises the following steps: providing a target material; depositing the amorphous thin film on a substrate by using a magnetron sputtering method.
4. The method of claim 3, wherein the amorphous thin film is formed by sputtering. The target material is selected from a composite material of Al and SiC.
5. The method of claim 4, wherein the amorphous thin film is formed by sputtering. In the composite material of Al and SiC, the mass ratio of Al to SiC is 3:
7.
6. The method of claim 3, wherein the amorphous thin film is formed by sputtering. In the step of magnetron sputtering, the radio frequency power applied during deposition is 500 W-600 W.
7. The method of claim 3, wherein the amorphous thin film is formed by sputtering. In the step of magnetron sputtering, the deposition pressure is 0.32 Pa-0.36 Pa.
8. The method of claim 3, wherein the amorphous thin film is formed by sputtering. In the step of magnetron sputtering, the deposition time is 7200 seconds-18000 seconds.
9. The amorphous thin film according to any one of claims 1-2 for use as a surface protection material.