CN113582172B - Diamond-like carbon structure and preparation method and application thereof - Google Patents

Diamond-like carbon structure and preparation method and application thereof Download PDF

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CN113582172B
CN113582172B CN202110808906.6A CN202110808906A CN113582172B CN 113582172 B CN113582172 B CN 113582172B CN 202110808906 A CN202110808906 A CN 202110808906A CN 113582172 B CN113582172 B CN 113582172B
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diamond
nitrogen
carbon structure
oxygen
vacuum chamber
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CN113582172A (en
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林海天
李立升
郑礼伟
陈松
杨恺
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Guangdong Huasheng Nanotechnology Co ltd
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Dongguan Huasheng Vacuum Plated Film Technology Co ltd
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/25—Diamond
    • C01B32/26—Preparation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0635—Carbides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C23C16/27—Diamond only
    • C23C16/278—Diamond only doping or introduction of a secondary phase in the diamond

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Abstract

The invention relates to the technical field of diamond-like carbon, in particular to a diamond-like carbon structure and a preparation method and application thereof. According to the invention, nitrogen element is doped in the diamond-like carbon structure, so that the concentration of current carriers in the diamond-like carbon structure is improved, the conductivity of the diamond-like carbon structure is improved, and meanwhile, oxygen element with the mass ratio of (1-10): 1 is doped, so that the concentration of the current carriers is further improved, the hydrogen content in the diamond-like carbon structure is reduced, and sp brought by nitrogen doping is balanced 2 The increase of the structure content avoids the reduction of mechanical properties such as hardness, strength and the like, expands the application scene of the diamond-like carbon structure, and particularly greatly improves the usability of the diamond-like carbon structure in the 3C electronic field.

Description

Diamond-like carbon structure and preparation method and application thereof
Technical Field
The invention relates to the technical field of diamond-like carbon, in particular to a diamond-like carbon structure and a preparation method and application thereof.
Background
With the development of the 3C electronic industry, the internal structure of a 3C electronic product is more and more complex, and the original structures such as a connecting rod and a rotor therein bear severe abrasion, so that the requirements on hardness, abrasion resistance and the like are high, and meanwhile, certain requirements on conductivity are also met. Therefore, the development of a high hardness coating having conductivity and wear resistance is of great commercial value.
The diamond-like coating has sp 2 And sp 3 Bonding mode of blending, wherein sp is similar to graphite 2 The structure has certain self-lubricating effect, can improve the wear resistance of the film layer, and is similar to sp of diamond 3 The structure can improve the mechanical properties of the material such as hardness, strength and the like, so that the diamond-like coating has excellent strength and wear resistance, but the conductivity of the diamond-like coating is higherPoor, cannot meet the conductive requirements of the 3C field. In order to solve the problem, in the traditional technology, the conductivity of the diamond-like carbon coating is improved by doping metal in the diamond-like carbon coating, but the friction coefficient of the diamond-like carbon coating is greatly increased after the diamond-like carbon coating is doped with metal, and the wear resistance is greatly reduced; in addition, methods have been developed to increase conductivity by doping nitrogen to increase the carrier concentration in the coating, but nitrogen doping can cause sp in diamond-like coatings 2 The increase of the structure content leads to the reduction of the mechanical property of the coating, so that the prepared coating has poor hardness and strength.
Disclosure of Invention
Based on this, there is a need for a diamond-like carbon structure, a preparation method and an application thereof, which can be used for preparing a diamond-like coating layer that not only meets the conductive requirements in the 3C field, but also maintains excellent mechanical properties.
According to one aspect of the invention, a diamond-like carbon structure is provided, wherein the diamond-like carbon structure is doped with nitrogen and oxygen in a mass ratio of (1-10): 1.
According to the invention, nitrogen element is doped in the diamond-like carbon structure, so that the concentration of current carriers in the diamond-like carbon structure is improved, the conductivity of the diamond-like carbon structure is improved, and meanwhile, oxygen element with the mass ratio of (1-10): 1 is doped, so that the concentration of the current carriers is further improved, the conductivity of the diamond-like carbon structure is further improved, the hydrogen content in the diamond-like carbon structure is reduced, and sp brought by nitrogen doping is balanced 2 Increase of structure content, thereby sp in diamond-like carbon structure 2 And sp 3 The content of the structure is maintained in a reasonable range, the reduction of mechanical properties such as hardness, strength and the like is avoided, the application scene of the diamond-like carbon structure is expanded, and particularly the usability of the diamond-like carbon structure in the 3C electronic field is greatly improved.
In some embodiments, the diamond-like carbon structure has a nitrogen content of 3% to 25% by weight.
In some embodiments, the diamond-like carbon structure has a nitrogen content of 11% to 20% by weight.
In some embodiments, the diamond-like carbon structure is a thin layer having a thickness of 200nm to 2000 nm.
In another aspect of the present invention, there is provided a method for preparing the aforementioned diamond-like carbon structure, comprising the steps of:
providing a substrate, and depositing a carbon source, a nitrogen source and an oxygen source on the substrate by a vapor deposition technique to form the diamond-like carbon structure.
In some embodiments, the vapor deposition technique is physical vapor deposition, the carbon source is methane and/or acetylene, the nitrogen source is nitrogen, and the oxygen source is oxygen.
In some embodiments, the physical vapor deposition has an ion source power of 500W to 3000W.
In some embodiments, the bias voltage for physical vapor deposition is a negative voltage with a value of 0V to 200V.
In some embodiments, the carbon source has a flow rate of 50sccm to 100 sccm.
In some embodiments, the total flow rate of the nitrogen and the oxygen is 50sccm to 100 sccm.
In some embodiments, the substrate is made of one or more of a simple metal, an alloy, a metal oxide, and a silicon wafer.
The invention also provides an electronic product which comprises the diamond-like carbon structure.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the accompanying examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the invention, "a plurality" means at least two, e.g., two, three, etc., unless explicitly specified otherwise. In the description of the present invention, "a plurality" means at least one, e.g., one, two, etc., unless specifically limited otherwise.
Unless defined otherwise, 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 belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In one aspect of the invention, a diamond-like carbon structure is provided, wherein nitrogen and oxygen are doped in a mass ratio of (1-10): 1.
Charge carriers are particles of a substance that carry a charge and are free to move to form an electric current. Semiconductors differ in their properties from conductors and insulators because of their different band structures; the conductivity of the semiconductor can be controlled mainly because the types and the quantity of the carriers are different from those of the conductor and the insulator, and the regulation means is doping, namely impurities are doped into the pure semiconductor to change the quantity, the distribution and the movement trend of the carriers, so that the overall conductivity is changed.
Similarly, for the diamond-like carbon structure with poor conductivity, the conductivity can be improved by doping nitrogen element which can obviously improve the concentration of carriers; however, in the conventional technology, when the doping amount of nitrogen reaches about 10% of the mass of the diamond-like carbon structure, sp is generated 2 The situation that the mechanical property is greatly reduced occurs due to the increase of the structural content, and the requirement of a high-conductivity scene is difficult to meet due to the nitrogen doping amount of only 10%. The doping of oxygen element into the diamond-like carbon structure can also increase the concentration of current carrier to a certain extent, thereby realizing the improvement of conductivity, however, the excessive doping of oxygen element can lead to the class The diamond carbon structure is oxidized and the performance of the diamond-like carbon structure is also greatly affected.
Through a large number of experiments, the inventor finds that after the doping amount of nitrogen is determined according to the requirement of the required electrical conductivity, if the mass ratio of nitrogen to the diamond-like carbon structure is (1-10): 1, nitrogen-oxygen co-doping is carried out on the diamond-like carbon structure, the diamond-like carbon structure can be maintained not to be oxidized, simultaneously, the hydrogen content in the diamond-like carbon structure is effectively reduced, and sp brought by nitrogen doping is counteracted 2 The increase of the structure content balances sp in the diamond-like carbon structure 2 And sp 3 The proportion of the structure is kept in a reasonable range, and the reduction of mechanical properties such as hardness, strength and the like of the diamond-like carbon structure is avoided; meanwhile, the concentration of a carrier can be improved to a certain extent by the doping of the oxygen element, so that the conductivity of the diamond-like carbon structure is further improved compared with that of single nitrogen doping after the diamond-like carbon structure is modified by nitrogen-oxygen co-doping in a reasonable proportion, the application scene of the diamond-like carbon structure is effectively expanded, and particularly the usability of the diamond-like carbon structure in the field of 3C electronics is greatly improved.
Preferably, the mass ratio of nitrogen element and oxygen element doped in the diamond-like carbon structure is (1.5-7): 1. Further preferably, the mass ratio of nitrogen element and oxygen element doped in the diamond-like carbon structure is (2-4): 1, such as 2.5: 1. The mass ratio of the nitrogen element to the oxygen element is maintained in a reasonable range, so that the conductivity and the mechanical property of the diamond-like carbon structure can be improved to the maximum extent.
In some embodiments, the content of nitrogen in the diamond-like carbon structure is 3% to 25% by mass. Preferably, the content of nitrogen element in the diamond-like carbon structure is 5-20% by mass. Further preferably, the content of nitrogen in the diamond-like carbon structure is 11% to 20% by mass, for example 12%, 13%, 14%, 15%, 16%, 17%, 18% or 19%.
In some embodiments, the total mass percent content of nitrogen and oxygen in the diamond-like carbon structure is between 10% and 30%. Preferably, the total mass percentage content is 12-22%. More preferably, the total mass percentage content is 15-21%.
When the nitrogen doping amount is low, the improvement on the electrical conductivity is limited, and the influence on the mechanical property of the diamond-like carbon structure is small, so that the improvement on the mechanical property by nitrogen-oxygen co-doping compared with single nitrogen doping is limited; when the nitrogen doping amount is higher, in order to reduce sp 2 The content of the structure and the doping amount of oxygen also need to be correspondingly increased, but when the doping amount of oxygen reaches a certain level, the diamond-like carbon structure is oxidized, so that the mechanical property is reduced, and therefore, the improvement of the mechanical property of the diamond-like carbon structure is limited no matter more or less oxygen is doped at the moment.
In some embodiments, the diamond-like carbon structure is a thin layer having a thickness of 200nm to 2000 nm. Alternatively, the thin layer may have a thickness of 300nm, 400nm, 500nm, 600nm, 700nm, 800nm, 900nm, 1000nm, 1100nm, 1200nm, 1300nm, 1400nm, 1500nm, 1600nm, 1700nm, 1800nm, 1900 nm. In a preset thickness range, nitrogen-oxygen co-doping can better improve the conductivity and mechanical property of the diamond-like carbon thin layer.
In another aspect of the present invention, there is provided a method for preparing the aforementioned diamond-like carbon structure, comprising the steps of:
providing a substrate, and depositing a carbon source, a nitrogen source and an oxygen source on the substrate by a vapor deposition technology to form a diamond-like carbon structure.
In some embodiments, the vapor deposition technique is chemical vapor deposition.
In some embodiments, the vapor deposition technique is physical vapor deposition, in which case the carbon source is methane and/or acetylene, the nitrogen source is nitrogen, and the oxygen source is oxygen.
In some embodiments, the physical vapor deposition technique is magnetron sputtering or arc ion plating; preferably, the ion source is an anode layer ion source.
In some embodiments, the ion source power for physical vapor deposition is 500W to 3000W. Alternatively, the ion source power may be, for example, 600W, 700W, 800W, 900W, 1000W, 1100W, 1200W, 1300W, 1400W, 1500W, 1600W, 1700W, 1800W, 1900W, 2000W, 2100W, 2200W, 2300W, 2400W, 2500W, 2600W, 2700W, 2800W, 2900W.
In some embodiments, the bias voltage for physical vapor deposition is a cathode voltage of a value of 0V to 200V.
In some embodiments, the current for physical vapor deposition is from 80A to 100A.
In some embodiments, the carbon source is flowed at a rate of 50sccm to 100 sccm.
In some embodiments, the total flow rate of nitrogen and oxygen is 50sccm to 100 sccm.
In some embodiments, the substrate is made of one or more of a simple metal, an alloy, a metal oxide, and a silicon wafer.
In some embodiments, a transition layer comprised of a metal or nonmetal and its carbide is deposited on the substrate prior to depositing the diamond-like carbon structure. The bonding force between the diamond-like carbon structure and the substrate can be effectively improved by depositing the transition layer.
In some embodiments, the transition layer is one or more of a chromium/chromium carbide transition layer, a titanium/titanium carbide transition layer, a tungsten/tungsten carbide transition layer, or a silicon/silicon carbide transition layer.
In some embodiments, the transition layer has a thickness of 100nm to 1000 nm.
In some embodiments, the substrate is cleaned prior to depositing the transition layer or the diamond-like carbon structure on the surface of the substrate, the cleaning including at least one of an organic solvent cleaning and an ion source cleaning. The organic solvent cleaning can remove oil stains, dust and other stains adsorbed on the surface of the substrate; ion source cleaning consistently and reliably removes contaminants from the substrate surface, activating the substrate surface and making it more susceptible to bonding to the deposited film layer.
In some embodiments, the organic solvent is an alcohol solvent such as ethanol or isopropanol.
Preferably, the organic solvent cleaning manner is ultrasonic cleaning.
Further preferably, the substrate is blow dried with a flow of dry air after the ultrasonic cleaning.
When performing ion source cleaning:
in some embodiments, the substrate is placed in a vacuum chamber and the pressure of the vacuum chamber is brought to less than 4 x 10 - 3 Pa, and then turning on an ion source for cleaning.
In some embodiments, during the cleaning with the ion source, a protective gas is introduced into the vacuum chamber, the vacuum chamber is evacuated while introducing the protective gas, and the pressure in the vacuum chamber is maintained at 0.1Pa to 1 Pa. Preferably, the pressure in the vacuum chamber is 0.8Pa to 1 Pa.
In some embodiments, the protective gas is at least one of argon, helium, and neon.
In some embodiments, the flow rate of the protective gas is between 300sccm and 400 sccm.
In some embodiments, the ion source power is set to 500W-1500W, and the cleaning time is 20 min-60 min.
In some embodiments, during the cleaning of the substrate, a bias voltage is applied to the substrate at a negative voltage having a value of 800V to 1000V.
In one specific example, arc ion plating is used for deposition, and an anode layer ion source is used; at this time, the preparation method of the diamond-like carbon structure includes the steps of:
(1) ultrasonically cleaning a substrate by using an organic solvent, rinsing the substrate by using deionized water, and drying the substrate by using dry compressed air; placing the cleaned and dried substrate on a workpiece support of a vacuum chamber, and vacuumizing to 4 × 10 -3 Below Pa, starting an ion source, introducing protective gas with the flow rate of 300 sccm-400 sccm into the vacuum chamber, maintaining the pressure of the vacuum chamber at 0.1 Pa-1 Pa, setting the power of the ion source at 500W-1500W, applying a negative electrode voltage with the value of 800V-1000V to the substrate, and cleaning for 20 min-60 min;
(2) introducing protective gas with the flow rate of 50 sccm-200 sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.1 Pa-1 Pa; starting an arc evaporation source loaded with a metal or nonmetal target material, setting the current of the arc evaporation source to be 80-100A, applying a negative voltage with a value of 0-200V to the substrate, and gradually introducing a gas carbon source until the flow of the gas carbon source reaches 200sccm and the thickness of a deposition transition layer is 100-1000 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 500-3000W, introducing a carbon source with the flow rate of 50-100 sccm, introducing a nitrogen source and an oxygen source with the total flow rate of 50-100 sccm, depositing a nitrogen-oxygen co-doped diamond-like coating with the thickness of 200-2000 nm under the negative voltage with the value of 0-200V, adjusting the total flow rate of the nitrogen source and the oxygen source to ensure that the doping amount of nitrogen elements in the prepared coating is 3-25%, and adjusting the flow ratio of the nitrogen source to the oxygen source to ensure that the mass ratio of the nitrogen elements to the oxygen elements in the prepared coating is (1-10): 1.
The invention also provides an electronic product which comprises the diamond-like carbon structure.
The present invention will be described in further detail with reference to specific examples and comparative examples. It is understood that the following examples are more specific to the apparatus and materials used, and in other embodiments, are not limited thereto.
Example 1
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the silicon wafer, and cleaning for 30 min;
(2) introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) Starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow rate of 100sccm, introducing high-purity nitrogen and high-purity oxygen with the total flow rate of 100sccm, depositing a nitrogen-oxygen co-doped diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V, adjusting the total flow rate of the nitrogen and the oxygen to enable the doping amount of nitrogen in the prepared coating to be 15%, and adjusting the flow ratio of the nitrogen to the oxygen to enable the mass ratio of the nitrogen to the oxygen in the prepared coating to be 2.5: 1;
(4) and (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
Example 2
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the silicon wafer, and cleaning for 30 min;
(2) introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow rate of 100sccm, introducing high-purity nitrogen and high-purity oxygen with the total flow rate of 100sccm, depositing a nitrogen-oxygen co-doped diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V, adjusting the total flow rate of the nitrogen and the oxygen to enable the doping amount of nitrogen in the prepared coating to be 8%, and adjusting the flow ratio of the nitrogen to the oxygen to enable the mass ratio of the nitrogen to the oxygen in the prepared coating to be 2.5: 1;
(4) and (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
Example 3
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the silicon wafer, and cleaning for 30 min;
(2) Introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow rate of 100sccm, introducing high-purity nitrogen and high-purity oxygen with the total flow rate of 100sccm, depositing a nitrogen-oxygen co-doped diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V, adjusting the total flow rate of the nitrogen and the oxygen to enable the doping amount of nitrogen in the prepared coating to be 21%, and adjusting the flow ratio of the nitrogen to the oxygen to enable the mass ratio of the nitrogen to the oxygen in the prepared coating to be 2.5: 1;
(4) and (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
Example 4
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting the ion source, introducing argon gas with the flow rate of 350sccm into the vacuum chamber, maintaining the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, and applying the value of 1000 to the silicon waferV, and washing for 30 min;
(2) introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow rate of 100sccm, introducing high-purity nitrogen and high-purity oxygen with the total flow rate of 100sccm, depositing a nitrogen-oxygen co-doped diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V, adjusting the total flow rate of the nitrogen and the oxygen to enable the doping amount of nitrogen in the prepared coating to be 15%, and adjusting the flow ratio of the nitrogen to the oxygen to enable the mass ratio of the nitrogen to the oxygen in the prepared coating to be 5: 1;
(4) and (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
Example 5
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the silicon wafer, and cleaning for 30 min;
(2) introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow rate of 100sccm, introducing high-purity nitrogen and high-purity oxygen with the total flow rate of 100sccm, depositing a nitrogen-oxygen co-doped diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V, adjusting the total flow rate of the nitrogen and the oxygen to enable the doping amount of nitrogen in the prepared coating to be 8%, and adjusting the flow ratio of the nitrogen to the oxygen to enable the mass ratio of the nitrogen to the oxygen in the prepared coating to be 1: 1;
(4) And (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
Example 6
(1) Ultrasonically cleaning a 304 stainless steel workpiece by using an organic solvent, rinsing the workpiece by using deionized water, and drying the workpiece by using dry compressed air; placing the cleaned and dried 304 stainless steel workpiece on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 - 3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the 304 stainless steel workpiece, and cleaning for 30 min;
(2) introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an electric arc evaporation source loaded with a chromium target, setting the current of the electric arc evaporation source to be 100A, simultaneously applying a negative electrode voltage with a value of 100V to the metal workpiece, introducing high-purity methane gradually until the flow of the high-purity methane reaches 200sccm, and depositing Cr/CrC x The thickness of the transition layer is 100 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 2000W, introducing high-purity methane with the flow rate of 50sccm, introducing high-purity nitrogen and high-purity oxygen with the total flow rate of 50sccm, depositing a nitrogen-oxygen co-doped diamond-like coating with the thickness of 200nm under the negative voltage with the value of 200V, adjusting the total flow rate of the nitrogen and the oxygen to enable the total doping amount of nitrogen elements in the prepared coating to be 20%, and adjusting the flow ratio of the nitrogen to the oxygen to enable the mass ratio of the nitrogen elements to the oxygen elements in the prepared coating to be 3: 1;
(4) And (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the 304 stainless steel workpiece with the diamond-like carbon structure.
Comparative example 1
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the silicon wafer, and cleaning for 30 min;
(2) introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow rate of 100sccm, introducing high-purity nitrogen with the flow rate of 100sccm, depositing a nitrogen-doped diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V, and adjusting the nitrogen flow rate to ensure that the doping amount of nitrogen elements in the prepared coating is 21 percent;
(4) And (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
Comparative example 2
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the silicon wafer, and cleaning for 30 min;
(2) introducing into the vacuum chamberArgon gas with the flow rate of 200sccm is adopted, and the whole pressure of the vacuum chamber is controlled to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow rate of 100sccm, introducing high-purity oxygen with the flow rate of 100sccm, depositing an oxygen-doped diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V, and adjusting the oxygen flow rate to ensure that the doping amount of oxygen elements in the prepared coating is 21 percent;
(4) And (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
Comparative example 3
(1) Ultrasonically cleaning a silicon wafer by using an organic solvent, rinsing the silicon wafer by using deionized water, and drying the silicon wafer by using dry compressed air; placing the cleaned and dried silicon wafer on a workpiece support of a vacuum chamber, and vacuumizing to 4 x 10 -3 Below Pa, starting an ion source, introducing argon gas with the flow of 350sccm into the vacuum chamber, keeping the pressure of the vacuum chamber at 0.6Pa, setting the power of the ion source at 1000W, applying a negative electrode voltage with the value of 1000V to the silicon wafer, and cleaning for 30 min;
(2) introducing argon gas with the flow rate of 200sccm into the vacuum chamber, and controlling the whole pressure of the vacuum chamber to be 0.6 Pa; starting an arc evaporation source loaded with a silicon target, setting the current of the arc evaporation source to be 100A, applying a negative electrode voltage with a value of 100V to a silicon wafer, introducing high-purity acetylene gradually until the flow of the high-purity acetylene reaches 200sccm, and depositing Si/SiC x The thickness of the transition layer is 600 nm;
(3) starting an anode layer ion source, setting the power of the anode layer ion source to be 1000W, introducing high-purity acetylene with the flow of 100sccm, and depositing a diamond-like coating with the thickness of 2000nm under the negative voltage with the value of 200V;
(4) And (4) turning off the power supply, opening the vacuum chamber after the temperature of the vacuum chamber is reduced to room temperature, and taking out the silicon wafer with the diamond-like carbon structure.
And (3) performance testing:
the diamond-like carbon structures prepared in the above examples and comparative examples were tested for friction coefficient (GB/T-10006-:
TABLE 1
Coefficient of friction hardness/HV 25 resistivity/K omega cm
Example 1 0.082 2100 0.22
Example 2 0.083 2120 0.66
Example 3 0.082 1550 0.20
Example 4 0.081 1830 0.28
Example 5 0.082 1580 0.54
Example 6 0.081 2050 0.25
Comparative example 1 0.081 1200 1.2
Comparative example 2 0.082 900 1.3
Comparative example 3 0.085 2150 40
As can be seen from Table 1, the diamond-like coating (comparative example 3) without any doping has a high hardness of 2150HV, but has a high resistivity of 40K Ω cm, and the conductivity is not sufficient to meet the requirements of 3C electronic field; if the coating is doped with 21% of nitrogen only (comparative example 1) or oxygen only (comparative example 2), although the resistance of the coating can be effectively reduced, the hardness of the coating is greatly reduced because the nitrogen doping causes sp in the coating 2 Too much structural content, hardThe degree drops to 1200HV, while oxygen doping causes the coating to oxidize, reducing the hardness even more, only 900 HV.
Under the condition of 21% of total doping amount, the resistivity is greatly reduced to 0.22K Ω · cm by nitrogen-oxygen co-doping in a reasonable proportion in the embodiment 1 on the premise of only reducing the hardness by 50HV, and the balance between the mechanical property and the electrical conductivity of the diamond-like coating is effectively realized. Nitrogen in example 2: the proportion of oxygen is unchanged, but the total doping amount is reduced to 11.2%, although the hardness has a weak advantage compared with that of the coating prepared in example 1, the resistivity is obviously increased, and the resistivity of 0.66K omega cm shows that the coating prepared in example 2 still has excellent conductivity; in the embodiment 3, the total doping amount is higher, the conductivity is slightly improved compared with the embodiment 1, the hardness is obviously reduced, and the actual use requirement is met; example 4 total doping was unchanged, but nitrogen: the oxygen proportion is improved compared with that of the embodiment 1, the oxygen content is slightly lower, and therefore, the hardness is reduced; example 5 total doping was unchanged, but nitrogen: the oxygen proportion is reduced compared with that of the embodiment 1, the oxygen content is slightly higher, the oxidation is caused to be extremely small, the hardness of the coating is obviously reduced, the conductivity is not good as that of the embodiment 1, and the overall performance is reduced.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the patent of the invention is subject to the appended claims, and the description can be used for explaining the contents of the claims.

Claims (11)

1. A diamond-like carbon structure is characterized in that the diamond-like carbon structure is doped with nitrogen and oxygen in a mass ratio of (1-10): 1, and the mass percentage of the nitrogen in the diamond-like carbon structure is 3% -25%.
2. A diamond-like carbon structure according to claim 1, characterized in that the content of nitrogen element in the diamond-like carbon structure is 11-20% by mass.
3. A diamond-like carbon structure according to any of claims 1-2, characterized in that the diamond-like carbon structure is a thin layer with a thickness of 200-2000 nm.
4. A method of preparing a diamond-like carbon structure according to any of claims 1 to 3 comprising the steps of:
providing a substrate, and depositing a carbon source, a nitrogen source and an oxygen source on the substrate by a vapor deposition technique to form the diamond-like carbon structure.
5. The method according to claim 4, wherein the vapor deposition technique is physical vapor deposition, the carbon source is methane and/or acetylene, the nitrogen source is nitrogen, and the oxygen source is oxygen.
6. The method according to claim 5, wherein the physical vapor deposition has an ion source power of 500 to 3000W.
7. The method according to claim 5, wherein the bias voltage of the physical vapor deposition is a negative electrode voltage having a value of 0V to 200V.
8. The method according to claim 5, wherein the flow rate of the carbon source is 50sccm to 100 sccm.
9. The production method according to claim 5, wherein a total flow rate of the nitrogen gas and the oxygen gas is 50sccm to 100 sccm.
10. The method according to any one of claims 4 to 9, wherein the substrate is made of one or more of a simple metal, an alloy, a metal oxide, and a silicon wafer.
11. An electronic product comprising the diamond-like carbon structure according to any one of claims 1 to 3.
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