Preparation method of high-ductility DLC film

Abstract

The invention discloses a preparation method of a high-ductility DLC film. The preparation method comprises the following steps: preparing an original DLC film; the original DLC film is placed in a vacuum chamber, and the vacuum degree in the vacuum chamber is kept to be not lower than 10 <-5 > Pa; spraying a solution containing silicon dioxide on the surface of the original DLC film to obtain a first DLC film; and carrying out annealing treatment on the first DLC film, and taking out the first DLC film from the vacuum chamber to obtain the treated DLC film. By the adoption of the technical scheme, the ductility and toughness of the DLC film can be improved under the condition that the hardness, abrasion resistance and other excellent performance of the DLC film are not damaged.

Description

Technical Field

[0001] The invention relates to the technical field of film preparation, and in particular to a method for preparing a DLC film with high ductility. Background Art

[0002] DLC (Diamond-like Carbon) film is a thin film composed of carbon and hydrogen elements. It has excellent mechanical properties, chemical stability and biocompatibility. Therefore, it is widely used in many fields, such as high-speed cutting, automobile and machine parts.

[0003] Although DLC film has excellent mechanical properties such as hardness and wear resistance, its chemical structure composed of carbon and hydrogen elements is relatively tight, resulting in relatively poor ductility and difficulty in adapting to certain complex stress field environments. Therefore, improving the ductility of DLC film is an important technical requirement.

[0004] In the prior art, in order to improve the ductility of the DLC film, methods such as sputtering or dissolving a thin film containing metal or non-metal elements on the surface of the DLC film are often used. The disadvantage of such methods is that it is difficult to obtain satisfactory results because an overly thick coating will destroy the excellent properties of the DLC film, such as hardness and wear resistance. Summary of the invention

[0005] The purpose of the embodiments of the present invention is to provide a method for preparing a DLC film with high ductility, which can improve the ductility and toughness of the DLC film without destroying the excellent properties of the DLC film, such as hardness and wear resistance.

[0006] In order to achieve the above object, an embodiment of the present invention provides a method for preparing a DLC film with high ductility, comprising:

[0007] Preparing a pristine DLC film;

[0008] The original DLC film is placed in a vacuum chamber, and the vacuum degree in the vacuum chamber is maintained at not less than 10 -5 Pa;

[0009] Spraying a solution containing silicon dioxide onto the surface of the original DLC film to obtain a first DLC film;

[0010] The first DLC film is subjected to annealing treatment and taken out from the vacuum chamber to obtain a treated DLC film.

[0011] Furthermore, the thickness of the original DLC film is 100 nm to 5 μm.

[0012] Furthermore, the hardness of the original DLC film is 15 GPa to 50 GPa.

[0013] Furthermore, the concentration of silicon dioxide in the solution is 3% to 5%.

[0014] Furthermore, the annealing temperature is 100°C to 300°C.

[0015] Furthermore, the annealing time is 60 min to 120 min.

[0016] Compared with the prior art, the embodiment of the present invention provides a method for preparing a DLC film with high ductility. First, an original DLC film is prepared; then, the original DLC film is placed in a vacuum chamber, and the vacuum degree in the vacuum chamber is maintained at not less than 10 -5 Pa; then, a solution containing silicon dioxide is sprayed on the surface of the original DLC film to obtain a first DLC film, and finally, the first DLC film is annealed and taken out from the vacuum chamber to obtain a treated DLC film. The embodiment of the present invention sprays a solution containing silicon dioxide on the surface of the DLC film and performs an annealing treatment, so that silicon dioxide can be infiltrated into the DLC film to increase the gap between its segments, thereby significantly improving the ductility and toughness of the DLC film without destroying the excellent properties of the DLC film, such as hardness and wear resistance. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a flow chart of a preferred embodiment of a method for preparing a high-ductility DLC film provided by the present invention. DETAILED DESCRIPTION

[0018] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this technical field without creative work are within the scope of protection of the present invention.

[0019] The present invention provides a method for preparing a DLC film with high ductility. Figure 1 FIG. 1 is a flow chart of a preferred embodiment of a method for preparing a high-ductility DLC film provided by the present invention, wherein the method comprises steps S11 to S14:

[0020] Step S11, preparing an original DLC film;

[0021] Step S12: placing the original DLC film in a vacuum chamber and maintaining the vacuum degree in the vacuum chamber to be not less than 10 - 5 Pa;

[0022] Step S13, spraying a solution containing silicon dioxide onto the surface of the original DLC film to obtain a first DLC film;

[0023] Step S14, annealing the first DLC film and taking it out from the vacuum chamber to obtain a treated DLC film.

[0024] In the specific implementation, first, an original DLC film is prepared, wherein the original DLC film can be prepared by an existing commonly used preparation method, such as ion beam deposition method, radio frequency magnetron sputtering method, etc. Then, the prepared original DLC film is placed in a vacuum chamber, and the vacuum degree in the vacuum chamber is maintained at not less than 10 -5 Pa; then, in a vacuum chamber, spray a solution containing silicon dioxide onto the surface of the original DLC film, select a solution of appropriate concentration and spray it evenly on the surface of the original DLC film, and accordingly obtain a first DLC film; finally, anneal the obtained first DLC film in a vacuum chamber, and take out the annealed first DLC film from the vacuum chamber, and accordingly obtain a treated DLC film, wherein the treated DLC film is a highly ductile DLC film, which can be used for subsequent processing or use, for example, surface functionalization or coating of other additional layers and other processing steps can be continued.

[0025] It should be noted that in the embodiment of the present invention, through annealing treatment, silicon dioxide can penetrate into the DLC film and fill its segment spacing, thereby improving the ductility and toughness of the DLC film, so that the highly ductile DLC film can also be well used in complex application scenarios.

[0026] It should be noted that, in the embodiment of the present invention, the solution containing silicon dioxide contains aerogel particles with a smaller particle size distribution, which can significantly improve the surface smoothness and density of the treated DLC film.

[0027] It can be understood that the embodiment of the present invention does not require complicated processing operations such as additional coating on the DLC film, so that the DLC film can obtain better application prospects.

[0028] In another preferred embodiment, the thickness of the original DLC film is 100 nm to 5 μm.

[0029] Specifically, in combination with the above embodiments, the thickness of the original DLC film prepared by adopting the existing commonly used preparation method is in the range of 100 nanometers to 5 micrometers.

[0030] In one of the optional embodiments, the thickness of the original DLC film is 1 μm to 5 μm.

[0031] Exemplarily, the thickness of the original DLC film can be 100nm, 200nm, 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1μm, 2μm, 3μm, 4μm or 5μm, and can also be set according to actual needs, which is not specifically limited in the embodiments of the present invention.

[0032] In yet another preferred embodiment, the hardness of the original DLC film is 15 GPa to 50 GPa.

[0033] Exemplarily, the hardness of the original DLC film can be 15 GPa, 20 GPa, 25 GPa, 30 GPa, 35 GPa, 40 GPa, 45 GPa or 50 GPa, and can also be set according to actual needs, which is not specifically limited in the embodiments of the present invention.

[0034] In yet another preferred embodiment, the concentration of silicon dioxide in the solution is 3% to 5%.

[0035] Specifically, in combination with the above-mentioned embodiment, the concentration of the silicon dioxide solution sprayed on the surface of the original DLC film is in the range of 3% to 5%.

[0036] It should be noted that the solution contains aerogel particles with a smaller particle size distribution, and the particle size is about 20 nanometers to 100 nanometers.

[0037] Exemplarily, the solution concentration may be 3%, 3.5%, 4%, 4.5% or 5%, and may also be set according to actual needs, which is not specifically limited in the embodiment of the present invention.

[0038] In yet another preferred embodiment, the annealing temperature is 100°C to 300°C.

[0039] Specifically, in combination with the above embodiment, when the first DLC film is annealed, the annealing temperature is in the range of 100°C to 300°C.

[0040] Exemplarily, the annealing temperature may be 100°C, 110°C, 120°C, 130°C, 140°C, 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, 290°C or 300°C, and may also be set according to actual needs, and the embodiments of the present invention are not specifically limited.

[0041] In another preferred embodiment, the annealing time is 60 min to 120 min.

[0042] Specifically, in combination with the above embodiment, when the first DLC film is annealed, the annealing time is in the range of 60 minutes to 120 minutes.

[0043] Exemplarily, the annealing time may be 60 minutes, 70 minutes, 80 minutes, 90 minutes, 100 minutes, 110 minutes or 120 minutes, and may also be set according to actual needs, which is not specifically limited in the embodiment of the present invention.

[0044] The surface morphology and mechanical properties of the treated DLC film were tested, and the test results are as follows:

[0045] (1) Surface morphology test: The surface of the DLC film after treatment changes significantly, and its surface smoothness and density are improved;

[0046] (2) Mechanical properties test: The hardness and wear resistance of the DLC film after treatment did not change significantly, while the ductility and toughness of the DLC film were significantly improved, with the ductility increasing from 1% to about 10%.

[0047] In combination with all the above embodiments, the implementation process of the present solution is described below through the first specific embodiment, including: (1) using ion beam deposition to prepare an original DLC film, wherein the thickness of the original DLC film is 100nm and the hardness is 15GPa; (2) placing the prepared original DLC film in a vacuum chamber and maintaining the vacuum degree in the vacuum chamber to be not less than 10 -5 Pa; (3) In a vacuum chamber, a solution containing silicon dioxide is sprayed onto the surface of the original DLC film, and a solution with a silicon dioxide concentration of 3% is selected to be evenly sprayed on the surface of the original DLC film, thereby obtaining a first DLC film; (4) The obtained first DLC film is annealed in a vacuum chamber at a temperature of 100°C and an annealing time of 60 min; (5) The annealed first DLC film is taken out of the vacuum chamber, thereby obtaining a treated DLC film.

[0048] In combination with all the above embodiments, the implementation process of the present solution is described below through a second specific embodiment, including: (1) preparing an original DLC film by ion beam deposition, wherein the thickness of the original DLC film is 3 μm and the hardness is 30 GPa; (2) placing the prepared original DLC film in a vacuum chamber, and maintaining the vacuum degree in the vacuum chamber not less than 10 -5Pa; (3) In a vacuum chamber, a solution containing silicon dioxide is sprayed onto the surface of the original DLC film, and a solution with a silicon dioxide concentration of 4% is selected to be evenly sprayed on the surface of the original DLC film, thereby obtaining a first DLC film; (4) The obtained first DLC film is annealed in a vacuum chamber at a temperature of 200°C and an annealing time of 90 min; (5) The annealed first DLC film is taken out of the vacuum chamber, thereby obtaining a treated DLC film.

[0049] In combination with all the above embodiments, the implementation process of the present solution is described below through a third specific embodiment, including: (1) preparing an original DLC film by ion beam deposition, wherein the thickness of the original DLC film is 5 μm and the hardness is 50 GPa; (2) placing the prepared original DLC film in a vacuum chamber, and maintaining the vacuum degree in the vacuum chamber to be not less than 10 -5 Pa; (3) In a vacuum chamber, a solution containing silicon dioxide is sprayed onto the surface of the original DLC film, and a solution with a silicon dioxide concentration of 5% is selected to be evenly sprayed on the surface of the original DLC film, thereby obtaining a first DLC film; (4) The obtained first DLC film is annealed in a vacuum chamber at a temperature of 300°C and an annealing time of 120 min; (5) The annealed first DLC film is taken out of the vacuum chamber, thereby obtaining a treated DLC film.

[0050] In summary, the method for preparing a DLC film with high ductility provided by the embodiment of the present invention comprises the following steps: first, preparing an original DLC film; then, placing the original DLC film in a vacuum chamber, and maintaining the vacuum degree in the vacuum chamber to be not less than 10 -5 Pa; then, a solution containing silicon dioxide is sprayed on the surface of the original DLC film to obtain a first DLC film, and finally, the first DLC film is annealed and taken out from the vacuum chamber to obtain a treated DLC film. The embodiment of the present invention sprays a solution containing silicon dioxide on the surface of the DLC film and performs an annealing treatment, so that silicon dioxide can be infiltrated into the DLC film to increase the gap between its segments, thereby significantly improving the ductility and toughness of the DLC film without destroying the excellent properties of the DLC film, such as hardness and wear resistance.

[0051] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the technical principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a high-ductility DLC film, characterized in that: include: Preparing a pristine DLC film; The original DLC film is placed in a vacuum chamber, and the vacuum degree in the vacuum chamber is maintained at not less than 10 -5 Pa; Spraying a solution containing silicon dioxide onto the surface of the original DLC film to obtain a first DLC film; The first DLC film is subjected to annealing treatment and taken out from the vacuum chamber to obtain a treated DLC film.

2. The method for preparing a highly ductile DLC film according to claim 1, wherein: The thickness of the original DLC film is 100 nm to 5 μm.

3. The method for preparing a highly ductile DLC film according to claim 1, characterized in that: The hardness of the original DLC film is 15 GPa to 50 GPa.

4. The method for preparing a highly ductile DLC film according to claim 1, wherein: The concentration of silicon dioxide in the solution is 3% to 5%.

5. The method for preparing a highly ductile DLC film according to claim 1, characterized in that: The annealing temperature is 100°C to 300°C.

6. The method for preparing a highly ductile DLC film according to claim 1, wherein: The annealing time is 60min~120min.

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