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; carrying out cleaning treatment on the surface of the original DLC film; and carrying out heat treatment on the cleaned DLC film at a preset temperature to obtain the high-ductility DLC film. According to the technical scheme, the ductility of the DLC film can be improved, and the effect is good.

Description

Technical Field

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

[0002] A DLC (Diamondlike Carbon) film is a hard thin film composed of carbon elements, which has excellent wear resistance, corrosion resistance and the characteristic of reducing the friction coefficient, so it is widely used in the fields of machinery, tools, automobiles, etc. However, due to the special structure and properties of the DLC film, its ductility is poor, and problems such as cracking and peeling are likely to occur, which are intolerable in some applications.

[0003] At present, many methods for improving the ductility of DLC films have been proposed. For example, by increasing the ductility of the underlying material adjacent to the DLC film to improve its overall ductility, or by using a nitrogen oxide mixed gas to prepare an oxygen-containing or nitrogen-containing DLC film. Although these existing methods can improve the ductility of the DLC film to a certain extent, they still have certain limitations and the effects are not good. Summary of the Invention

[0004] 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 of the DLC film and has better effects.

[0005] To achieve the above purpose, the embodiments of the present invention provide a method for preparing a DLC film with high ductility, including:

[0006] Preparing an original DLC film;

[0007] Cleaning the surface of the original DLC film;

[0008] Performing heat treatment on the cleaned DLC film at a preset temperature to obtain a DLC film with high ductility.

[0009] Further, the preparation of the original DLC film specifically includes:

[0010] Preparing an original DLC film on a substrate by chemical vapor deposition under a preset medium pressure.

[0011] Further, the preparation of the original DLC film on a substrate by chemical vapor deposition under a preset medium pressure specifically includes:

[0012] Preparing an original DLC film on a substrate by chemical vapor deposition at a medium pressure of 1.3 kPa, using C2H2 and CH4 as carbon sources, Ar as a dilution and inert gas, and H2 as a carrier gas.

[0013] Further, the cleaning treatment of the surface of the original DLC film specifically includes:

[0014] The surface of the original DLC film is cleaned by chemical bath or plasma cleaning method.

[0015] Further, the heat treatment of the cleaned DLC film at a preset temperature to obtain a highly ductile DLC film specifically includes:

[0016] Place the cleaned DLC film in a high-temperature furnace;

[0017] Heat the cleaned DLC film to the preset temperature and maintain it at the preset temperature for a preset time for heat treatment;

[0018] Cool the heat-treated DLC film to room temperature to obtain a highly ductile DLC film.

[0019] Further, the heating of the cleaned DLC film to the preset temperature specifically includes:

[0020] Heat the cleaned DLC film in air at a rate of 1 °C / min to 500 °C - 800 °C.

[0021] Further, the preset time is 1 - 4 h.

[0022] Compared with the prior art, the embodiment of the present invention provides a method for preparing a highly ductile DLC film. First, an original DLC film is prepared; then, the surface of the original DLC film is cleaned; finally, the cleaned DLC film is heat-treated at a preset temperature to obtain a highly ductile DLC film. By performing high-temperature heat treatment on the DLC film, the carbide bonds in the DLC film are broken, thereby improving the ductility of the DLC film with better effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 is a flowchart of a preferred embodiment of a method for preparing a highly ductile DLC film provided by the present invention. DETAILED DESCRIPTION

[0024] The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art in this technical field without creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.

[0025] An embodiment of the present invention provides a method for preparing a DLC film with high ductility. Refer to Figure 1 As shown in the flowchart of a preferred embodiment of a method for preparing a DLC film with high ductility provided by the present invention, the method includes steps S11 to S13:

[0026] Step S11, prepare the original DLC film;

[0027] Step S12, clean the surface of the original DLC film;

[0028] Step S13, perform heat treatment on the cleaned DLC film at a preset temperature to obtain a DLC film with high ductility.

[0029] In specific implementation, first, prepare the original DLC film; then, clean the surface of the prepared original DLC film to remove impurities on the surface of the original DLC film and obtain the cleaned DLC film; finally, perform high-temperature heat treatment on the cleaned DLC film at a preset temperature to obtain a DLC film with high ductility.

[0030] It should be noted that for the DLC film after high-temperature treatment, after the fracture force test, it is found that it is more ductile than the untreated DLC film, and the peel resistance and wear resistance are also improved.

[0031] In one alternative embodiment, the preparation of the original DLC film specifically includes:

[0032] Prepare the original DLC film on the substrate by chemical vapor deposition under a preset medium pressure.

[0033] Specifically, in combination with the above embodiment, when preparing the original DLC film, the original DLC film can be formed on the substrate by chemical vapor deposition under a preset medium pressure.

[0034] It should be noted that in actual preparation of the original DLC film, any suitable substrate can be selected. For example, the substrate used can be glass, quartz, or metal, etc.

[0035] Exemplarily, in the embodiment of the present invention, the original DLC film can be grown on a SiO2 glass substrate by chemical vapor deposition.

[0036] In one alternative embodiment, the preparation of the original DLC film on the substrate by chemical vapor deposition under a preset medium pressure specifically includes:

[0037] Under a medium pressure of 1.3 kPa, using C2H2 and CH4 as carbon sources, Ar as a diluting and inert gas, and H2 as a carrier gas, an original DLC film is prepared on a substrate by chemical vapor deposition.

[0038] Specifically, in combination with the above embodiments, in the process of preparing the original DLC film by chemical vapor deposition, under a preset medium pressure, C2H2 and CH4 can be used as carbon sources, Ar can be used as a diluting and inert gas, and H2 can be used as a carrier gas, and the original DLC film can be grown on the substrate by chemical vapor deposition, and the total reaction pressure during the growth process is 1.3 kPa.

[0039] In one alternative embodiment, the cleaning treatment of the surface of the original DLC film specifically includes:

[0040] The surface of the original DLC film is cleaned by chemical bath or plasma cleaning method.

[0041] Specifically, in combination with the above embodiments, when cleaning the surface of the original DLC film, any suitable surface cleaning process can be adopted. For example, the surface of the original DLC film can be cleaned by chemical bath or plasma cleaning method.

[0042] In one alternative embodiment, the heat treatment of the cleaned DLC film at a preset temperature to obtain a highly ductile DLC film specifically includes:

[0043] Place the cleaned DLC film in a high-temperature furnace;

[0044] Heat the cleaned DLC film to the preset temperature and maintain it at the preset temperature for a preset time for heat treatment;

[0045] Cool the heat-treated DLC film to room temperature to obtain a highly ductile DLC film.

[0046] Specifically, in combination with the above embodiments, when heat-treating the cleaned DLC film at a high temperature, the cleaned DLC film can be first placed in a high-temperature furnace, and the cleaned DLC film can be heated in the high-temperature furnace to heat the cleaned DLC film to the preset temperature and maintain it at the preset temperature for a preset time for heat treatment; then the heat-treated DLC film is cooled to cool the heat-treated DLC film to room temperature, and a highly ductile DLC film is correspondingly obtained.

[0047] It should be noted that in actual heat treatment, in addition to using a high-temperature furnace as a heating device, other devices that can provide an appropriate temperature can also be used in the embodiments of the present invention, such as a heat treatment furnace or a plasma furnace, etc.

[0048] In one alternative embodiment, heating the cleaned DLC film to a preset temperature specifically includes:

[0049] Heating the cleaned DLC film in air at a rate of 1 °C / min to 500 °C - 800 °C.

[0050] Specifically, in combination with the above embodiment, the preset temperature is 500 °C - 800 °C. That is, when heating the DLC film after cleaning treatment, the cleaned DLC film can be heated to 500 °C - 800 °C. Further, the cleaned DLC film can be heated in air at a rate of 1 °C / min to 500 °C - 800 °C.

[0051] Exemplarily, the value of the preset temperature can be 500 °C, 550 °C, 600 °C, 650 °C, 700 °C, 750 °C or 800 °C, or it can be set according to actual requirements, and the embodiments of the present invention do not make specific limitations.

[0052] In one alternative embodiment, the preset time is 1 - 4 h.

[0053] Specifically, in combination with the above embodiment, the preset time is 1 hour to 4 hours. That is, after heating the DLC film after cleaning treatment to the preset temperature, it is maintained at this preset temperature for 1 hour to 4 hours.

[0054] It should be noted that during the heat treatment process, the DLC film must be heated to a temperature of 500 °C - 800 °C and maintained at this temperature for 1 hour to 4 hours to ensure that the DLC film is completely heat-treated and strengthened.

[0055] Exemplarily, the value of the preset time can be 1 hour, 1 hour 30 minutes, 2 hours, 2 hours 30 minutes, 3 hours, 3 hours 30 minutes or 4 hours, or it can be set according to actual requirements, and the embodiments of the present invention do not make specific limitations.

[0056] As a preferred solution, when heat-treating the cleaned DLC film at high temperature, the cleaned DLC film can be heated in air at a rate of 1 °C / min to 650 °C and kept at 650 °C for 4 hours.

[0057] Combining all the above embodiments, the implementation process of this solution is described below through the first specific embodiment, including: (1) Under a preset medium pressure, using C2H2 and CH4 as carbon sources, using Ar as a dilution and inert gas, using H2 as a carrier gas, a raw DLC film is prepared on a substrate by chemical vapor deposition, and the total reaction pressure during the growth of the raw DLC film is 1.3 kPa; (2) The surface of the raw DLC film is cleaned by chemical bath or plasma cleaning method to obtain a cleaned DLC film; (3) The cleaned DLC film is placed in a high-temperature furnace, and the cleaned DLC film is heat-treated in the high-temperature furnace by heating the cleaned DLC film in air at a rate of 1 °C / min to 500 °C and maintaining it at 500 °C for 1 hour for heat treatment; (4) The heat-treated DLC film is cooled to obtain a highly ductile DLC film at room temperature.

[0058] Combining all the above embodiments, the implementation process of this solution is described below through the second specific embodiment, including: (1) Under a preset medium pressure, using C2H2 and CH4 as carbon sources, using Ar as a dilution and inert gas, using H2 as a carrier gas, a raw DLC film is prepared on a substrate by chemical vapor deposition, and the total reaction pressure during the growth of the raw DLC film is 1.3 kPa; (2) The surface of the raw DLC film is cleaned by chemical bath or plasma cleaning method to obtain a cleaned DLC film; (3) The cleaned DLC film is placed in a high-temperature furnace, and the cleaned DLC film is heat-treated in the high-temperature furnace by heating the cleaned DLC film in air at a rate of 1 °C / min to 650 °C and maintaining it at 650 °C for 2 hours and 30 minutes for heat treatment; (4) The heat-treated DLC film is cooled to obtain a highly ductile DLC film at room temperature.

[0059] Combining all the above embodiments, the implementation process of this solution is described below through a third specific embodiment, including: (1) Under a pre-set medium pressure, using C2H2 and CH4 as carbon sources, using Ar as a dilution and inert gas, using H2 as a carrier gas, a raw DLC film is prepared on a substrate by chemical vapor deposition, and the total reaction pressure during the growth of the raw DLC film is 1.3 kPa; (2) The surface of the raw DLC film is cleaned by chemical bath or plasma cleaning method to obtain a cleaned DLC film; (3) The cleaned DLC film is placed in a high-temperature furnace, and the cleaned DLC film is heat-treated in the high-temperature furnace by heating the cleaned DLC film in air at a rate of 1 °C / min to 800 °C and maintaining it at 800 °C for 4 hours for heat treatment; (4) The heat-treated DLC film is cooled to room temperature to obtain a highly ductile DLC film.

[0060] In summary, for a method for preparing a highly ductile DLC film provided by an embodiment of the present invention, first, a raw DLC film is prepared; then, the surface of the raw DLC film is cleaned; finally, the cleaned DLC film is heat-treated at a preset temperature to obtain a highly ductile DLC film. By subjecting the DLC film to high-temperature heat treatment, the carbide bonds in the DLC film are broken, thereby improving the ductility of the DLC film, and the effect is better.

[0061] In addition, heat treatment also helps to improve the peel resistance and wear resistance of the DLC film. Further, the embodiments of the present invention can be easily implemented and can be quickly and easily applied to the existing DLC film preparation process, so it has a wide application prospect.

[0062] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the technical principle of the present invention, several improvements and deformations can be made, and these improvements and deformations should also be regarded as the protection scope of the present invention.

Claims

1. A preparation method of a highly ductile DLC film, characterized in that, Including: Preparing an original DLC film; Performing a cleaning treatment on the surface of the original DLC film; Performing a heat treatment on the cleaned DLC film at a preset temperature to obtain a highly ductile DLC film.

2. The method for preparing a highly ductile DLC film according to claim 1, characterized in that, The preparation of the original DLC film specifically includes: Preparing an original DLC film on a substrate by chemical vapor deposition under a preset medium pressure.

3. The method for preparing a highly ductile DLC film according to claim 2, characterized in that, The preparation of the original DLC film on a substrate by chemical vapor deposition under a preset medium pressure specifically includes: Preparing an original DLC film on a substrate by chemical vapor deposition under a medium pressure of 1.3 kPa, using C2H2 and CH4 as carbon sources, Ar as a dilution and inert gas, and H2 as a carrier gas.

4. The method for preparing a highly ductile DLC film according to claim 1, characterized in that, The performing a cleaning treatment on the surface of the original DLC film specifically includes: Performing a cleaning treatment on the surface of the original DLC film by chemical bath or plasma cleaning method.

5. The preparation method of the highly ductile DLC film according to claim 1, characterized in that, The performing a heat treatment on the cleaned DLC film at a preset temperature to obtain a highly ductile DLC film specifically includes: Placing the cleaned DLC film in a high-temperature furnace; Heating the cleaned DLC film to a preset temperature and maintaining it at the preset temperature for a preset time for heat treatment; Cooling the heat-treated DLC film to room temperature to obtain a highly ductile DLC film.

6. The method for preparing a highly ductile DLC film according to claim 5, characterized in that, The heating the cleaned DLC film to a preset temperature specifically includes: Heating the cleaned DLC film in air at a rate of 1 °C / min to 500 °C - 800 °C.

7. The method for preparing a highly ductile DLC film according to claim 5, characterized in that, The preset time is 1 - 4 h.

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