Preparation method of high-flexibility DLC film

Abstract

The invention discloses a preparation method of a high-flexibility DLC (Diamond Like Carbon) film, which comprises the following steps: placing a film coating substrate on a rotating frame in a vacuum chamber, adjusting the air pressure in the vacuum chamber to be 1.5 * 10 <-2 > Pa, and adjusting the rotating speed of the rotating frame to be 80r / min; and depositing a DLC film on the surface of the coating substrate, and doping a gaseous polyurethane monomer with the DLC film after a preset deposition time so as to form the high-flexibility DLC film on the surface of the coating substrate. By adopting the technical scheme of the invention, the low-rigidity and high-flexibility DLC film can be prepared, so that the film layer is effectively prevented from brittle rupture and falling off, and a hole-sealable film layer can be deposited on the surface of the DLC film, so that the performance of the DLC film is improved.

Description

Technical Field

[0001] This invention relates to the field of thin film preparation technology, and in particular to a method for preparing a highly flexible DLC film. Background Technology

[0002] With the development of technology, DLC (Diamond-like Carbon) films are widely used in various fields due to their advantages in the following aspects: 1. Super hardness: DLC films have higher hardness than metals, effectively protecting the coated surface from scratches, wear, and other damage; 2. High wear resistance: DLC films have excellent wear resistance, extending the service life of the coated material; 3. Corrosion resistance: DLC films have excellent corrosion resistance, maintaining the integrity of the coated surface in harsh environments; 4. Reduced coefficient of friction: Adding DLC ​​films to the surface of parts can reduce the coefficient of friction and improve the movement efficiency of the parts; 5. Ultra-low friction: Under certain conditions, DLC films can also exhibit ultra-low friction performance, reducing energy loss; 6. Excellent texture.

[0003] However, DLC films prepared using existing technologies have good rigidity but insufficient flexibility, making them prone to brittleness. Furthermore, as DLC films become thinner, micropores appear on their surface, allowing corrosive media to easily enter the substrate and corrode it, thus significantly reducing the performance of the film. Summary of the Invention

[0004] The purpose of this invention is to provide a method for preparing a highly flexible DLC film, which can produce a DLC film with low rigidity and high flexibility, thereby effectively preventing the film layer from cracking and falling off, and can deposit a pore-sealing film layer on the surface of the DLC film, thereby improving the performance of the DLC film.

[0005] To achieve the above objectives, embodiments of the present invention provide a method for preparing a highly flexible DLC film, comprising:

[0006] The coating substrate is placed on a rotating frame inside the vacuum chamber, and the air pressure inside the vacuum chamber is adjusted to 1.5 × 10⁻⁶. -2 Pa, adjust the rotation speed of the rotating frame to 80 r / min;

[0007] A DLC film is deposited on the surface of the coating substrate, and after a preset deposition time, gaseous polyurethane monomers are doped with the DLC film to form a highly flexible DLC film on the surface of the coating substrate.

[0008] Furthermore, the method also includes:

[0009] The polyurethane monomer is heated to 200-220°C to turn it into a gaseous state.

[0010] Further, the deposition of a DLC film on the surface of the coating substrate specifically involves:

[0011] A high-purity graphite target is activated, and a DLC film is deposited on the surface of the coating substrate under the conditions of a substrate bias voltage of 40-50V and a current of 2.5-3.0A for the high-purity graphite target.

[0012] Furthermore, the deposition time is 20–25 min.

[0013] Furthermore, the doping of the gaseous polyurethane monomer with the DLC film specifically involves:

[0014] Gaseous polyurethane monomers are introduced into the vacuum chamber using hydrocarbon gases, and the gas pressure inside the vacuum chamber is adjusted to 0.2–0.4 Pa.

[0015] A pulse bias voltage greater than 500V is applied to the coating substrate, and the working voltage of the ion beam is set to be greater than 800V and the working current is 100-150mA, so that polyurethane monomers are doped in the DLC film.

[0016] Furthermore, the flow rate of the gaseous polyurethane monomer is 20–30 sccm.

[0017] Furthermore, the doping time of the gaseous polyurethane monomer with the DLC film is 20 to 30 minutes.

[0018] Furthermore, the thickness of the highly flexible DLC film is 15 μm.

[0019] Compared with the prior art, the present invention provides a method for preparing a highly flexible DLC film. First, the coating substrate is placed on a rotating frame inside a vacuum chamber, and the air pressure inside the vacuum chamber is adjusted to 1.5 × 10⁻⁶. -2 Pa, adjust the rotation speed of the rotating frame to 80 r / min; then, deposit a DLC film on the surface of the coating substrate, and after a preset deposition time, dope the DLC film with gaseous polyurethane monomers to form a highly flexible DLC film on the surface of the coating substrate. This invention can prepare a low-rigidity, highly flexible DLC film on the surface of the coating substrate, effectively preventing film brittleness and peeling, and can deposit a pore-sealing film layer on the surface of the DLC film, thereby improving the performance of the DLC film. Attached Figure Description

[0020] Figure 1This is a flowchart of a preferred embodiment of a method for preparing a highly flexible DLC film provided by the present invention. Detailed Implementation

[0021] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] This invention provides a method for preparing a highly flexible DLC film, see [link to relevant documentation]. Figure 1 The diagram shown is a flowchart of a preferred embodiment of a method for preparing a highly flexible DLC film provided by the present invention, the method comprising steps S11 to S12:

[0023] Step S11: Place the coating substrate on the rotating frame inside the vacuum chamber, and adjust the air pressure inside the vacuum chamber to 1.5 × 10⁻⁶. -2 Pa, adjust the rotation speed of the rotating frame to 80 r / min;

[0024] Step S12: Deposit a DLC film on the surface of the coating substrate, and after a preset deposition time, dope the DLC film with gaseous polyurethane monomers to form a highly flexible DLC film on the surface of the coating substrate.

[0025] In practice, the coating substrate is first placed on a rotating frame inside the vacuum chamber, and the internal air pressure of the vacuum chamber is adjusted and maintained at 1.5 × 10⁻⁶. -2 Pa, and adjust the rotation speed of the rotating frame to 80 rpm; then, use plasma polymerization deposition technology to deposit a DLC film on the surface of the coating substrate, and after a preset deposition time, dope the pre-obtained gaseous polyurethane monomer with the DLC film deposited on the surface of the coating substrate, thereby forming a highly flexible DLC film on the surface of the coating substrate.

[0026] It should be noted that by doping gaseous polyurethane monomers with the DLC film, polyurethane monomers can be formed in the DLC film, thereby reducing the rigidity of the DLC film and improving its flexibility. At the same time, a pore-sealing film layer can be deposited on the surface of the DLC film, thereby improving the performance of the DLC film and extending its service life.

[0027] In one alternative embodiment, the method further includes:

[0028] The polyurethane monomer is heated to 200-220°C to turn it into a gaseous state.

[0029] Specifically, in conjunction with the above embodiments, the embodiments of the present invention can preheat polyurethane monomers in a heating tank to raise the temperature to 200°C to 220°C, thereby turning the polyurethane monomers into a gaseous state.

[0030] For example, the temperature after heating can be 200℃, 201℃, 202℃, 203℃, 204℃, 205℃, 206℃, 207℃, 208℃, 209℃, 210℃, 211℃, 212℃, 213℃, 214℃, 215℃, 216℃, 217℃, 218℃, 219℃ or 220℃, and can also be set according to actual needs. This embodiment of the invention does not make specific limitations.

[0031] In one optional embodiment, the deposition of the DLC film on the surface of the coating substrate specifically involves:

[0032] A high-purity graphite target is activated, and a DLC film is deposited on the surface of the coating substrate under the conditions of a substrate bias voltage of 40-50V and a current of 2.5-3.0A for the high-purity graphite target.

[0033] Specifically, in conjunction with the above embodiments, when depositing a DLC film on the surface of the coating substrate, a bias voltage of 40V to 50V can be applied to the coating substrate, and the current of the high-purity graphite target can be set to 2.5A to 3.0A. Under these parameter conditions, the high-purity graphite target is activated to deposit and form a DLC film on the surface of the coating substrate.

[0034] For example, when depositing a DLC film on the surface of the coating substrate, the bias voltage applied to the coating substrate can be 40V, 41V, 42V, 43V, 44V, 45V, 46V, 47V, 48V, 49V or 50V, and can also be set according to actual needs. This embodiment of the invention does not make specific limitations.

[0035] For example, when depositing a DLC film on the surface of the coating substrate, the current of the high-purity graphite target can be 2.5A, 2.6A, 2.7A, 2.8A, 2.9A or 3.0A, or can be set according to actual needs. This embodiment of the invention does not make specific limitations.

[0036] In one optional embodiment, the deposition time is 20 to 25 minutes.

[0037] Specifically, in conjunction with the above embodiments, the preset deposition time can be 20 min to 25 min. That is, when depositing a DLC film on the surface of the coating substrate, after 20 min to 25 min, the pre-obtained gaseous polyurethane monomer can be doped with the DLC film deposited on the surface of the coating substrate.

[0038] For example, the deposition time can be 20 minutes, 21 minutes, 22 minutes, 23 minutes, 24 minutes or 25 minutes, and can also be set according to actual needs. This embodiment of the invention does not make specific limitations.

[0039] In one optional embodiment, the doping of the gaseous polyurethane monomer with the DLC film specifically involves:

[0040] Gaseous polyurethane monomers are introduced into the vacuum chamber using hydrocarbon gases, and the gas pressure inside the vacuum chamber is adjusted to 0.2–0.4 Pa.

[0041] A pulse bias voltage greater than 500V is applied to the coating substrate, and the working voltage of the ion beam is set to be greater than 800V and the working current is 100-150mA, so that polyurethane monomers are doped in the DLC film.

[0042] Specifically, in conjunction with the above embodiments, when doping gaseous polyurethane monomers with DLC films, hydrocarbon gases can be used to carry the gaseous polyurethane monomers into a vacuum chamber. After introducing the polyurethane monomer gas into the vacuum chamber, the gas pressure in the vacuum chamber is adjusted to 0.2 Pa to 0.4 Pa, and a pulse bias voltage greater than 500 V is applied to the coating substrate. The working voltage applied to the ion beam is set to be greater than 800 V, and the working current applied to the ion beam is set to be 100 mA to 150 mA. Under these parameter conditions, the gaseous polyurethane monomers are doped with the DLC film deposited on the surface of the coating substrate to form polyurethane monomer doping in the DLC film.

[0043] For example, the adjusted air pressure in the vacuum chamber can be 0.2 Pa, 0.3 Pa, or 0.4 Pa, and can also be set according to actual needs. This embodiment of the invention does not impose specific limitations.

[0044] For example, the working current applied to the ion beam can be 100mA, 105mA, 110mA, 115mA, 120mA, 125mA, 130mA, 135mA, 140mA, 145mA or 150mA, and can also be set according to actual needs. This embodiment of the invention does not make specific limitations.

[0045] In one alternative embodiment, the flow rate of the gaseous polyurethane monomer is 20–30 sccm.

[0046] Specifically, in conjunction with the above embodiments, when using hydrocarbon gases to carry gaseous polyurethane monomers into the vacuum chamber, the flow rate of the gaseous polyurethane monomers is 20 sccm to 30 sccm.

[0047] For example, the flow rate of gaseous polyurethane monomers can be 20 sccm, 21 sccm, 22 sccm, 23 sccm, 24 sccm, 25 sccm, 26 sccm, 27 sccm, 28 sccm, 29 sccm or 30 sccm, and can also be set according to actual needs. This embodiment of the invention does not make specific limitations.

[0048] In one optional embodiment, the doping time of the gaseous polyurethane monomer with the DLC film is 20 to 30 minutes.

[0049] Specifically, in conjunction with the above embodiments, when doping the gaseous polyurethane monomer with the DLC film, the doping time of the gaseous polyurethane monomer with the DLC film is 20 min to 30 min. That is, firstly, a DLC film is deposited on the surface of the coating substrate for 20 min to 25 min. After 20 min to 25 min, the pre-obtained gaseous polyurethane monomer is then doped with the DLC film deposited on the surface of the coating substrate for 20 min to 30 min, thereby forming a highly flexible DLC film on the surface of the coating substrate.

[0050] For example, the doping time can be 20 minutes, 21 minutes, 22 minutes, 23 minutes, 24 minutes, 25 minutes, 26 minutes, 27 minutes, 28 minutes, 29 minutes or 30 minutes, and can also be set according to actual needs. This embodiment of the invention does not make specific limitations.

[0051] In one alternative embodiment, the thickness of the highly flexible DLC film is 15 μm.

[0052] Specifically, in conjunction with the above embodiments, the thickness of the finally prepared highly flexible DLC film is 15 μm. That is, firstly, a DLC film is deposited on the surface of the coating substrate, and then gaseous polyurethane monomers are doped with the DLC film to form a highly flexible DLC film with a thickness of 15 micrometers on the surface of the coating substrate.

[0053] Based on all the above embodiments, the implementation process of this solution is described below through the first specific embodiment, including: (1) preheating the polyurethane monomer in a heating tank to raise the temperature to 200°C, so that the polyurethane monomer becomes gaseous; (2) placing the coating substrate on a rotating frame inside the vacuum chamber, adjusting and maintaining the internal air pressure of the vacuum chamber at 1.5 × 10⁻⁶. -2 Pa, and adjust the rotation speed of the rotating frame to 80 rpm; (3) Using plasma polymerization deposition technology, apply a bias voltage of 40V to the coating substrate, and set the current of the high-purity graphite target to 2.5A. Under these parameters, start the high-purity graphite target to deposit a DLC film on the surface of the coating substrate, and the deposition time of the DLC film is 25min; (4) After a deposition time of 25min, use hydrocarbon gas to bring the gaseous polyurethane monomer into the vacuum chamber. At this time, the flow rate of the gaseous polyurethane monomer is 20sccm; (5) In the vacuum After introducing polyurethane monomer gas into the chamber, the pressure in the vacuum chamber is adjusted to 0.2 Pa, and a pulse bias voltage greater than 500 V is applied to the coating substrate. The working voltage applied to the ion beam is set to be greater than 800 V, and the working current applied to the ion beam is set to 100 mA. Under these parameters, the gaseous polyurethane monomer is doped with the DLC film deposited on the surface of the coating substrate for 30 min to form polyurethane monomer doping in the DLC film, thereby forming a highly flexible DLC film with a thickness of 15 micrometers on the surface of the coating substrate.

[0054] Based on all the above embodiments, the implementation process of this solution is described below through a second specific embodiment, including: (1) preheating the polyurethane monomer in a heating tank to a temperature of 210°C, causing the polyurethane monomer to become gaseous; (2) placing the coating substrate on a rotating frame inside the vacuum chamber, adjusting and maintaining the internal air pressure of the vacuum chamber at 1.5 × 10⁻⁶. -2Pa, and adjust the rotation speed of the rotating frame to 80 rpm; (3) Using plasma polymerization deposition technology, apply a bias voltage of 45V to the coating substrate, and set the current of the high-purity graphite target to 2.8A. Under these parameters, start the high-purity graphite target to deposit a DLC film on the surface of the coating substrate, and the deposition time of the DLC film is 22min; (4) After a deposition time of 22min, use hydrocarbon gas to bring the gaseous polyurethane monomer into the vacuum chamber. At this time, the flow rate of the gaseous polyurethane monomer is 25sccm; (5) In the vacuum After introducing polyurethane monomer gas into the chamber, the pressure in the vacuum chamber is adjusted to 0.3 Pa, and a pulse bias voltage greater than 500 V is applied to the coating substrate. The working voltage applied to the ion beam is set to be greater than 800 V, and the working current applied to the ion beam is set to 125 mA. Under these parameters, the gaseous polyurethane monomer is doped with the DLC film deposited on the surface of the coating substrate for 25 min to form polyurethane monomer doping in the DLC film, thereby forming a highly flexible DLC film with a thickness of 15 micrometers on the surface of the coating substrate.

[0055] Based on all the above embodiments, the implementation process of this solution is described below through a third specific embodiment, including: (1) preheating the polyurethane monomer in a heating tank to a temperature of 220°C, causing the polyurethane monomer to become gaseous; (2) placing the coating substrate on a rotating frame inside a vacuum chamber, adjusting and maintaining the internal air pressure of the vacuum chamber at 1.5 × 10⁻⁶. -2 Pa, and adjust the rotation speed of the rotating frame to 80 rpm; (3) Using plasma polymerization deposition technology, apply a bias voltage of 50V to the coating substrate, and set the current of the high-purity graphite target to 3.0A. Under these parameters, start the high-purity graphite target to deposit a DLC film on the surface of the coating substrate, and the deposition time of the DLC film is 20min; (4) After a deposition time of 20min, use hydrocarbon gas to bring the gaseous polyurethane monomer into the vacuum chamber. At this time, the flow rate of the gaseous polyurethane monomer is 30sccm; (5) In the vacuum After introducing polyurethane monomer gas into the chamber, the gas pressure in the vacuum chamber is adjusted to 0.4 Pa, and a pulse bias voltage greater than 500 V is applied to the coating substrate. The working voltage applied to the ion beam is set to be greater than 800 V, and the working current applied to the ion beam is set to 150 mA. Under these parameters, the gaseous polyurethane monomer is doped with the DLC film deposited on the surface of the coating substrate for 20 min to form polyurethane monomer doping in the DLC film, thereby forming a highly flexible DLC film with a thickness of 15 micrometers on the surface of the coating substrate.

[0056] In summary, the method for preparing a highly flexible DLC film provided by the embodiments of the present invention first involves placing the coating substrate on a rotating frame within a vacuum chamber and adjusting the gas pressure within the vacuum chamber to 1.5 × 10⁻⁶. -2 Pa, adjust the rotation speed of the rotating frame to 80 r / min; then, deposit a DLC film on the surface of the coating substrate, and after a preset deposition time, dope the DLC film with gaseous polyurethane monomers to form a highly flexible DLC film on the surface of the coating substrate. This invention can prepare a low-rigidity, highly flexible DLC film on the surface of the coating substrate, effectively preventing film brittleness and peeling, and can deposit a pore-sealing film layer on the surface of the DLC film, thereby improving the performance of the DLC film and extending its service life.

[0057] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the technical principles of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing a highly flexible DLC membrane, characterized in that, include: The coating substrate is placed on a rotating frame inside the vacuum chamber, and the air pressure inside the vacuum chamber is adjusted to 1.5 × 10⁻⁶. - 2 Pa, adjust the rotation speed of the rotating frame to 80 r / min; A DLC film is deposited on the surface of the coating substrate, and after a preset deposition time, gaseous polyurethane monomers are doped with the DLC film to form a highly flexible DLC film on the surface of the coating substrate.

2. The method for preparing the highly flexible DLC film as described in claim 1, characterized in that, The method further includes: The polyurethane monomer is heated to 200-220°C to turn it into a gaseous state.

3. The method for preparing the highly flexible DLC film as described in claim 1, characterized in that, The deposition of a DLC film on the surface of the coating substrate specifically involves: A high-purity graphite target is activated, and a DLC film is deposited on the surface of the coating substrate under the conditions of a substrate bias voltage of 40-50V and a current of 2.5-3.0A for the high-purity graphite target.

4. The method for preparing the highly flexible DLC film as described in claim 3, characterized in that, The deposition time is 20–25 min.

5. The method for preparing the highly flexible DLC film as described in claim 1, characterized in that, The process of doping the gaseous polyurethane monomer with the DLC film specifically involves: Gaseous polyurethane monomers are introduced into the vacuum chamber using hydrocarbon gases, and the gas pressure inside the vacuum chamber is adjusted to 0.2–0.4 Pa. A pulse bias voltage greater than 500V is applied to the coating substrate, and the working voltage of the ion beam is set to be greater than 800V and the working current is 100-150mA, so that polyurethane monomers are doped in the DLC film.

6. The method for preparing the highly flexible DLC film as described in claim 5, characterized in that, The flow rate of the gaseous polyurethane monomer is 20–30 sccm.

7. The method for preparing the highly flexible DLC film as described in claim 5, characterized in that, The doping time of the gaseous polyurethane monomer with the DLC film is 20-30 minutes.

8. The method for preparing a highly flexible DLC film according to any one of claims 1 to 7, characterized in that, The thickness of the highly flexible DLC film is 15 μm.

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