CN114196913B - Ultralow-friction solid-liquid composite lubricating coating and preparation method thereof - Google Patents

Ultralow-friction solid-liquid composite lubricating coating and preparation method thereof Download PDF

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CN114196913B
CN114196913B CN202111521225.8A CN202111521225A CN114196913B CN 114196913 B CN114196913 B CN 114196913B CN 202111521225 A CN202111521225 A CN 202111521225A CN 114196913 B CN114196913 B CN 114196913B
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diamond
coating
solid phase
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substrate
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CN114196913A (en
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李晓伟
乔江浩
冯存傲
蔡子明
吉祥
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China University of Mining and Technology CUMT
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    • 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
    • C23C14/0605—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/02—Hydrocarbon polymers; Hydrocarbon polymers modified by oxidation
    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • 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
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment

Abstract

The invention discloses an ultralow-friction solid-liquid composite lubricating coating and a preparation method thereof, and belongs to the technical field of material surface coating. The diamond-like coating is arranged on the friction surfaces of two or more substrates with mutual friction working conditions, and a lubricating oil layer serving as an intermediate liquid phase is arranged between the two or more substrates with mutual friction working conditions; the diamond-like carbon coating is only hydrogenated on the surface, and the atomic percentage of H element contained on the hydrogenated surface is 3% -38%. The diamond-like carbon solid phase has high hardness, good toughness and bearing performance, and the formed solid-liquid composite lubricating coating has extremely low friction coefficient (0-0.01) and wear rate, so that the diamond-like carbon solid phase is a composite lubricating coating material with excellent comprehensive performance, long service life and high reliability.

Description

Ultralow-friction solid-liquid composite lubricating coating and preparation method thereof
Technical Field
The invention relates to a lubricating coating and a preparation method thereof, in particular to an ultralow-friction solid-liquid composite lubricating coating and a preparation method thereof, which are applicable to industrial and mining enterprises and belong to the technical field of material surface coating.
Background
In recent years, the high-technology industries such as ocean, aviation, automobiles and micro-electromechanical industry rapidly develop, mechanical key moving parts face serious friction and abrasion problems, and particularly under the dual pressures of energy sources and environments, the traditional lubricating grease materials or single-component and single-structure solid lubricating coatings are difficult to meet the requirements of wear resistance, lubrication and bearing performance under the conditions of complex, changeable and severe working conditions (temperature, humidity, pressure, load, materials and the like), and research and development of new generation high-performance lubricating materials and lubricating technologies with the characteristics of ultralow friction, high bearing capacity, long service life, good environmental suitability and the like are urgently needed, so that the novel high-performance lubricating materials and lubricating technologies are key ways for prolonging the service lives of parts, realizing reliable operation, saving energy and reducing consumption.
Diamond-like carbon (DLC) is mainly composed of sp 3 Bond (diamond phase) and sp 2 The three-dimensional cross network of the bond (graphite phase) is mixed, has the characteristics of high hardness, low friction coefficient, good wear resistance, corrosion resistance, biocompatibility and the like, is used as an optimal surface modified solid lubricating material for key moving parts, becomes one of the hot spots which are paid attention to in the twenty-first century, can be successfully obtained under the environment-friendly and dry low-temperature physical/chemical vapor deposition technology, and meets the national important strategic requirements of energy conservation, consumption reduction and emission reduction.
However, in DLC basic research and engineering applications, there are mainly the following problems: (1) the residual stress is large, the film base binding force is poor, and the bonding with soft metal is especially weak; (2) the lubricating performance is greatly influenced by the ambient atmosphere (temperature, humidity, pressure, medium and the like); (3) the lubrication effect is inferior to that of fluid lubrication, and the friction coefficient is almost several times to tens times higher than that of grease lubrication; (4) self-consumption type lubrication has a certain limit on service life, so that the wide application and industrialization promotion of DLC solid lubrication materials are greatly limited.
The composite structure design and control of DLC material and the composite synergistic lubrication technology of lubricating oil, additive and the like are effective ways for solving the key technology and application bottleneck, prolonging the service life of the parts, realizing reliable operation, saving energy and reducing consumption. However, friction and abrasion are closely related to the surface/interface structure of the material, and the combination and interface optimization of coating materials with different structures generate different surface/interface structures, so that the friction characteristics of the coating and the basic physicochemical characteristics of adsorption, wetting and the like of lubricating oil and additives on the surface are affected.
Therefore, how to realize the synergistic lubrication of DLC and lubricating oil by the design and the regulation of the surface/interface structure of the DLC solid phase, develop high-performance solid-liquid composite lubricating materials and technologies, and are one of important research contents in the field of tribology and also the field of very active and active novel carbon functional materials.
Disclosure of Invention
Aiming at the defects of the prior art, the ultra-low friction solid-liquid composite lubricating coating which is easy to prepare, beneficial to industrial application and good in lubricating effect and the preparation method thereof are provided.
The invention provides a solid-liquid composite lubricating coating, which is a diamond-like coating arranged on two or more substrates with mutual friction working conditions, wherein the diamond-like coating is particularly arranged on the friction surfaces of the substrates, and a lubricating oil layer serving as an intermediate liquid phase is arranged between the two or more substrate diamond-like coatings with mutual friction working conditions; wherein the diamond-like carbon coating is only hydrogenated on the surface, and the atomic percentage of H element contained on the solid phase surface of the diamond-like carbon coating is 3% -38%; the H atoms on the solid phase surface of the diamond-like carbon coating and the H atoms in the lubricating oil layer are used for repulsive interaction, so that the distribution of lubricating oil and the physical and chemical adsorption action of the lubricating oil on the solid phase surface of the diamond-like carbon layer are influenced, in addition, the passivation action of the H element on a friction interface is improved, the antifriction lubricating performance between two or more substrates with diamond-like carbon layers on the surfaces is also improved, meanwhile, the extrusion action of the excessive hydrogenation of the solid phase surface of the diamond-like carbon coating on the lubricating oil is prevented, and the friction resistance between the substrates is increased.
The matrix material of the matrix provided with the diamond-like carbon coating comprises a hard alloy material, a steel material, an aluminum alloy material, a magnesium alloy material and a titanium alloy material.
The lubricating oil used in the lubricating oil layer comprises polyolefin, synthetic ester, polyalkyl ether, polysiloxane, alkylated aromatic/cyclic hydrocarbon and perfluoropolyether, and the liquid phase thickness of the lubricating oil layer is 0-100 nm.
The diamond-like layer disposed on the substrate being of a general sp 2 、sp 3 The amorphous carbon material composed of the hybridized structure only contains C, H two constituent elements on the solid phase surface of the diamond-like carbon coating; the thickness of the diamond-like carbon layer disposed on the substrate is 0.1 to 4 μm.
A preparation method of an ultralow-friction solid-liquid composite lubricating coating comprises the following steps:
a, etching and cleaning the surface of a substrate needing to prepare the composite lubricating coating by adopting an ion source and Ar gas as working gas sources so as to remove impurities on the surface of the substrate;
b, performing composite hydrogenation modification post-treatment by using magnetron sputtering to prepare a diamond-like coating with hydrogenated surface on the surface of the substrate; the specific process is as follows: firstly, starting a magnetron sputtering source, selecting high-purity graphite as a sputtering target material, introducing argon into the magnetron sputtering source, preparing a non-hydrogen diamond-like solid phase, then, switching off the magnetron sputtering source, switching on an ion source, and using H 2 For working gas source, the surface of non-hydrogen diamond-like solid phase is hydrogenated and modified by changing H 2 Controlling the flow rate and the atomic percentage content of H element on the surface of the pre-prepared diamond-like solid phase, thereby preparing a diamond-like coating with hydrogenated surface on the substrate;
further, the ion source operating current used in step a is 0.2A, the operating power is 200 to 350W, and the negative bias to the substrate is 100V.
Further, in step b, the negative bias voltage to the substrate is 50 to 150V.
In the step b, in the magnetron sputtering deposition method for the substrate, the power of the magnetron sputtering target is 0.9-1.6 KW, and the working current is 1.5-3A.
Further, in the method of the hydrogenation modification post-treatment of the step b, the temperature of the hydrogenation surface modification treatment is controlled to be 600K or less, H 2 The flow rate is 4.5-42 sccm.
The beneficial effects are that:
firstly, the coating comprises a diamond-like solid phase and a lubricating oil liquid phase, wherein the diamond-like solid phase has high hardness and excellent physical and chemical properties such as wear resistance lubrication, corrosion resistance, bearing and the like, and the self-consumption of the diamond-like solid phase can be remarkably reduced by adding the fluid lubrication behavior of the lubricating oil, so that the friction performance is synergistically improved; secondly, in the composite lubricating coating, the atomic percentage of H element on the self-assembled diamond-like solid phase surface is 3-38%, because the repulsive interaction exists between H atoms on the diamond-like solid phase surface and H atoms in lubricating oil, the distribution of the lubricating oil and the physical and chemical adsorption action of the lubricating oil on the diamond-like solid phase surface are affected, and the passivation action of H on a friction interface is added, so that the antifriction lubricating performance is optimal (the friction coefficient is between 0 and 0.01), and meanwhile, the phenomenon that the excessive hydrogenation on the diamond-like solid phase surface produces the extrusion action on the lubricating oil to increase the friction resistance can be avoided. Third, in the composite lubricating coating, the diamond-like solid phase only contains C, H two constituent elements, thereby avoiding the generation of frictional wear induced by corrosion of the solid phase during friction. Fourth, the composite lubricating coating has a wider application range of the matrix, and comprises hard alloy, various steels, aluminum alloy, magnesium alloy, titanium alloy and the like; for the matrix used under the complex and changeable working conditions of rich, lean, oil-free and the like, has excellent friction stability, prolonged service life and reliability.
The preparation method of the solid-liquid composite lubricating coating has the following advantages:
firstly, the deposition by adopting the magnetron sputtering composite hydrogenation modified post-treatment method can realize large-area uniform low-temperature deposition of the diamond-like solid phase with hydrogenated surface, and the operation is simple and easy to control, thereby being beneficial to industrial application. Secondly, in the magnetron sputtering composite hydrogenation modification post-treatment method, the temperature of the surface modification treatment is controlled below 600K, the intrinsic mechanical properties of the diamond-like carbon solid phase are not damaged while the surface is hydrogenated, and the comprehensive performance is optimal. Third, H is adopted 2 As a working air source, the accurate regulation and control of the contents of different H elements on the surface of the diamond-like carbon solid phase are realized by adjusting the air source flow.
Drawings
FIG. 1 is a graph showing the comparison of friction coefficients of solid-liquid composite lubricating coating samples obtained in example 1 and comparative examples 1-2;
FIG. 2 is a graph showing the comparison of friction coefficients of the solid-liquid composite lubricating coating samples obtained in example 2 and comparative examples 1-2;
FIG. 3 is a graph showing the comparison of friction coefficients of the solid-liquid composite lubricating coating samples prepared in example 3 and comparative examples 1-2;
Detailed Description
Embodiments of the invention are further described below with reference to the accompanying drawings:
the invention provides a solid-liquid composite lubricating coating, which consists of diamond-like carbon and lubricating oil. Wherein, the diamond-like carbon is used as self-matched upper and lower solid phases, and the lubricating oil is used as an intermediate liquid phase. In friction, the diamond-like solid phase has high hardness and excellent physical and chemical properties such as wear resistance, corrosion resistance, bearing and the like, and the friction performance is synergistically improved by adding the fluid lubrication behavior of lubricating oil. The ultra-low friction solid-liquid composite lubricating coating is a diamond-like coating arranged on two or more substrates with mutual friction working conditions, specifically the diamond-like coating is arranged on a friction contact surface of the substrates, and a lubricating oil layer serving as an intermediate liquid phase is arranged between the two or more substrate diamond-like coatings with mutual friction working conditions; wherein the diamond-like carbon coating is only hydrogenated on the surface, and the atomic percentage of H element contained on the solid phase surface of the diamond-like carbon coating is 3% -38%; the H atoms on the solid phase surface of the diamond-like carbon coating and the H atoms in the lubricating oil layer have repulsive interaction, so that the distribution of the lubricating oil and the physical and chemical adsorption action of the lubricating oil on the solid phase surface of the diamond-like carbon coating are influenced, and in addition, the passivation action of the H element on a friction interface is utilized, so that the antifriction lubricating performance is optimal. The antifriction and lubrication performance between two or more substrates with diamond-like carbon layers on the surfaces is improved, meanwhile, excessive hydrogenation of the solid phase surfaces of the diamond-like carbon coatings is prevented from producing extrusion action on lubricating oil, and the friction resistance between the substrates is increased.
The friction coefficient of the coating is between 0 and 0.01.
The matrix of the coating is hard alloy, various steels, aluminum alloy, magnesium alloy, titanium alloy and the like.
The liquid phase of the coating is a polyolefin, a synthetic ester, a polyalkylether, a polysiloxane, an alkylated aromatic/cyclic hydrocarbon, a perfluoropolyether, or the like.
The thickness of the liquid phase of the coating is 0-100 nm.
The diamond-like solid phase of the coating is a broad sp 2 、sp 3 The amorphous carbon material composed of the hybrid structure is generally called, and only the solid phase surface contains C, H two constituent elements.
The thickness of the diamond-like solid phase of the coating is 0.1-4 mu m.
Compared with the prior art, the solid-liquid composite lubricating coating has the following advantages:
first, because the coating comprises a diamond-like solid phase and a lubricating oil liquid phase, the diamond-like solid phase has high hardness and excellent physical and chemical properties such as wear resistance lubrication, corrosion resistance, bearing and the like, and the self-consumption of the diamond-like solid phase can be obviously reduced by adding the fluid lubrication behavior of the lubricating oil, and the friction performance can be synergistically improved. Secondly, in the composite lubricating coating, the atomic percentage of H element on the self-assembled diamond-like solid phase surface is 3% -38%, because the repulsive interaction exists between H atoms on the diamond-like solid phase surface and H atoms in lubricating oil, the distribution of the lubricating oil and the physical and chemical adsorption action of the lubricating oil on the diamond-like solid phase surface are affected, and the passivation action of H on a friction interface is added, so that the antifriction lubricating performance is optimal (the friction coefficient is between 0 and 0.01), and meanwhile, the phenomenon that the excessive hydrogenation on the diamond-like solid phase surface produces extrusion action on the lubricating oil to increase the friction resistance can be avoided. Third, in the composite lubricating coating, the diamond-like solid phase only contains C, H two constituent elements, thereby avoiding the generation of frictional wear induced by corrosion of the solid phase during friction. Fourth, the composite lubricating coating has a wider application range of the matrix, and comprises hard alloy, various steels, aluminum alloy, magnesium alloy, titanium alloy and the like; for the matrix used under the complex and changeable working conditions of rich, lean, oil-free and the like, has excellent friction stability, prolonged service life and reliability.
The invention also provides a preparation method of the solid-liquid composite lubricating coating, which comprises the following steps:
(1) Providing a substrate, and etching and cleaning the substrate by adopting an ion source and Ar gas as a working gas source;
(2) And (3) performing composite hydrogenation modification post-treatment by adopting magnetron sputtering to prepare the diamond-like carbon solid phase with hydrogenated surface.
In step (1), the object of the etching and cleaning of the substrate is to remove surface impurities on the one hand and to enlarge the surface of the substrate and to increase the adhesion between the diamond-like solid phase and the substrate on the other hand. The process specifically comprises the following steps: and etching and cleaning the substrate by adopting Ar gas plasma, wherein the working current of an ion source is 0.2A, the working power is 200-350W, and the negative bias voltage of the substrate is set to be 100V.
In the step (2), a magnetron sputtering composite hydrogenation modification post-treatment method is adopted to prepare a diamond-like solid phase, and the technological process and parameters are as follows: the magnetron sputtering source is a graphite target, argon is introduced into the magnetron sputtering source to prepare the hydrogen-free diamond-like carbon, and then the magnetron sputtering source is closed, the ion source is opened, and H is used 2 Performing surface hydrogenation modification for a working gas source, and controlling the atomic percentage content of H element on the surface of a solid phase by changing the flow of hydrogen; the power of the magnetron sputtering target is 0.9-1.6 KW, the working current is 1.5-3A, and the negative bias voltage of the substrate is 50-150V; the temperature of the hydrogenated surface modification treatment is controlled below 600K, H 2 The flow rate is 4.5-42 sccm.
The preparation method of the solid-liquid composite lubricating coating has the following advantages:
firstly, the deposition by adopting the magnetron sputtering composite hydrogenation modified post-treatment method can realize large-area uniform low-temperature deposition of the diamond-like solid phase with hydrogenated surface, and the operation is simple and easy to control, thereby being beneficial to industrial application. Secondly, in the magnetron sputtering composite hydrogenation modification post-treatment method, the temperature of the surface modification treatment is controlled below 600K, the intrinsic mechanical properties of the diamond-like carbon solid phase are not damaged while the surface is hydrogenated, and the comprehensive performance is optimal. Third, H is adopted 2 The method is characterized in that the method is used as a working air source, and the accurate regulation and control of the contents of different H elements on the diamond-like solid phase surface are realized by adjusting the air source flow
The tough wear-resistant coating and the preparation method thereof are described below with reference to specific examples:
example 1:
(1) Placing the substrate after ultrasonic cleaning on a vacuum chamber workpiece bracket;
(2) To adjust the pressure of the vacuum chamber to 2.7X10 -3 Pa, starting a linear ion source, introducing 40sccm argon into the linear ion source, wherein the working current of the linear ion source is 0.2A, the working power is 280W, and simultaneously setting the negative bias of a substrate to be 100V, and cleaning and etching a substrate for 15min;
(3) Deposition of diamond-like solid phase on substrate surface
Starting a magnetron sputtering source, and preparing a hydrogen-free diamond-like solid phase: the magnetron sputtering source is a high-purity graphite target (purity is larger than or equal to 99.99%), argon is introduced into the magnetron sputtering source, the gas flow is 50sccm, the power of the magnetron sputtering target is 1350W, the working current is 2.8A, meanwhile, the negative bias of the substrate is set to be 50V, the working air pressure is kept at 0.46Pa, and the deposition time is 1 hour. Then, the magnetron sputtering source is closed, the ion source is opened, and H is introduced 2 The working gas source is a working gas source, the gas flow is 30sccm, the working current of the ion source is 0.2A, and the working power is 250W; the negative bias of the substrate is set to 50V; the substrate heating temperature was 400K.
(4) And when the temperature of the vacuum chamber is reduced to room temperature, opening the cavity, and taking out the matrix, wherein the surface of the matrix is the diamond-like solid phase with hydrogenated surface.
(5) The diamond-like carbon prepared by the method is respectively used as an upper solid phase and a lower solid phase of the composite coating, polyolefin is selected as lubricating oil, and the lubricating oil is added into a friction interface of the upper solid phase and the lower solid phase to form the solid-liquid composite lubricating coating.
In the prepared solid-liquid composite lubricating coating obtained through test analysis, the thickness of the upper diamond-like carbon solid phase and the lower diamond-like carbon solid phase is 0.8 mu m, and the atomic percentage content of the surface H element is 18.8 percent and 18.8 percent respectively; the thickness of the polyolefin lubricant is 5nm. The friction coefficient of the coating was 0.007 at a contact pressure of 5GPa as shown in FIG. 1.
Example 2:
(1) Placing the substrate after ultrasonic cleaning on a vacuum chamber workpiece bracket;
(2) To adjust the pressure of the vacuum chamber to 2.7X10 -3 Pa, starting a linear ion source, introducing 40sccm argon into the linear ion source, wherein the working current of the linear ion source is 0.2A, the working power is 280W, and simultaneously setting the negative bias of a substrate to be 100V, and cleaning and etching a substrate for 15min;
(3) Deposition of diamond-like solid phase on substrate surface
Starting a magnetron sputtering source, and preparing a hydrogen-free diamond-like solid phase: the magnetron sputtering source is a high-purity graphite target (purity is larger than or equal to 99.99%),argon is introduced into the magnetron sputtering source, the gas flow is 50sccm, the power of the magnetron sputtering target is 1350W, the working current is 2.8A, meanwhile, the negative bias of the substrate is set to be 50V, the working air pressure is kept at 0.46Pa, and the deposition time is 1 hour. Then, the magnetron sputtering source is closed, the ion source is opened, and H is introduced 2 The working gas source is a working gas source, the gas flow is 35sccm, the working current of the ion source is 0.2A, and the working power is 260W; the negative bias of the substrate is set to 50V; the substrate heating temperature was 400K.
(4) And when the temperature of the vacuum chamber is reduced to room temperature, opening the cavity, and taking out the matrix, wherein the surface of the matrix is the diamond-like solid phase with hydrogenated surface.
(5) The diamond-like carbon prepared above was used as the lower solid phase of the composite coating.
(6) Repeating the steps (1) to (4), and changing the introduced H only in the surface hydrogenation modification treatment of the step (3) 2 The gas flow was 5sccm and the diamond-like carbon was prepared as the upper solid phase of the composite coating.
(7) The polyolefin is selected as lubricating oil, and is added to a friction interface formed by upper and lower solid phases of the prepared diamond-like carbon to form a solid-liquid composite lubricating coating.
In the prepared solid-liquid composite lubricating coating obtained through test analysis, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are 0.8 mu m, and the atomic percentage contents of the surface H elements are 3.6% and 24.9% respectively; the thickness of the polyolefin lubricant is 5nm. The friction coefficient of the coating at a contact pressure of 5GPa was 0.003, as shown in FIG. 2.
Example 3:
(1) Placing the substrate after ultrasonic cleaning on a vacuum chamber workpiece bracket;
(2) To adjust the pressure of the vacuum chamber to 2.7X10 -3 Pa, starting a linear ion source, introducing 40sccm argon into the linear ion source, wherein the working current of the linear ion source is 0.2A, the working power is 280W, and simultaneously setting the negative bias of a substrate to be 100V, and cleaning and etching a substrate for 15min;
(3) Deposition of diamond-like solid phase on substrate surface
Starting a magnetron sputtering source, and preparing a hydrogen-free diamond-like solid phase: magnetic control splashThe source is a high-purity graphite target (purity is not less than 99.99%), argon is introduced into the magnetron sputtering source, the gas flow is 50sccm, the power of the magnetron sputtering target is 1350W, the working current is 2.8A, the negative bias of the substrate is set to be 50V, the working air pressure is kept at 0.46Pa, and the deposition time is 1 hour. Then, the magnetron sputtering source is closed, the ion source is opened, and H is introduced 2 The working gas source is a working gas source, the gas flow is 40sccm, the working current of the ion source is 0.2A, and the working power is 280W; the negative bias of the substrate is set to 50V; the substrate heating temperature was 400K.
(4) And when the temperature of the vacuum chamber is reduced to room temperature, opening the cavity, and taking out the matrix, wherein the surface of the matrix is the diamond-like solid phase with hydrogenated surface.
(5) The diamond-like carbon prepared above was used as the lower solid phase of the composite coating.
(6) Repeating the steps (1) to (4), and changing the introduced H only in the surface hydrogenation modification treatment of the step (3) 2 The gas flow was 30sccm and the diamond-like carbon was prepared as the upper solid phase of the composite coating.
(7) The polyolefin is selected as lubricating oil, and is added to a friction interface formed by upper and lower solid phases of the prepared diamond-like carbon to form a solid-liquid composite lubricating coating.
In the prepared solid-liquid composite lubricating coating obtained through test analysis, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are 0.8 mu m, and the atomic percentage contents of surface H elements are 18.8% and 34.1% respectively; the thickness of the polyolefin lubricant is 5nm. The friction coefficient of the coating was 0.003 at a contact pressure of 5GPa as shown in fig. 3.
Comparative example 1:
this example is a comparative example of examples 1, 2, and 3 described above.
In this example, the preparation method of the solid-liquid composite lubricating coating was basically the same as that of example 1, except that in step (3), after the hydrogen-free diamond-like solid phase was prepared in advance, the ion source was not turned on to carry out the surface hydrogenation modification treatment, and the other process steps were the same as that of example 1.
In the prepared solid-liquid composite lubricating coating obtained through test analysis, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are 0.8 mu m, and the atomic percentage contents of the surface H elements are 0% and 0% respectively; the thickness of the polyolefin lubricant is 5nm. The friction coefficient of the coating under the contact pressure of 5GPa is 0.024 through friction test, as shown in figures 1, 2 and 3.
Comparative example 2:
this example is a comparative example of examples 1, 2, and 3 described above.
In this example, the method for preparing the solid-liquid composite lubricating coating was substantially the same as in example 1, except that in step (3), the hydrogen-free diamond-like solid phase was subjected to surface hydrogenation modification treatment, and H was introduced 2 The gas flow was 45sccm and the other process steps were the same as in example 1.
In the prepared solid-liquid composite lubricating coating obtained through test analysis, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are 0.8 mu m, and the atomic percentage contents of surface H elements are 44.1 percent and 44.1 percent respectively; the thickness of the polyolefin lubricant is 5nm. The friction coefficient of the coating under the contact pressure of 5GPa is 0.042 after friction test, as shown in figures 1, 2 and 3.

Claims (8)

1. An ultra-low friction solid-liquid composite lubricating coating is characterized in that: the diamond-like carbon coating is arranged on two or more substrates with mutual friction working conditions, specifically, the diamond-like carbon coating is arranged on the friction surfaces of the substrates with mutual friction, and a lubricating oil layer serving as an intermediate liquid phase is arranged between the two or more substrates with mutual friction working conditions; wherein the diamond-like carbon coating is only hydrogenated on the surface, and the atomic percentage of H element contained on the solid phase surface of the diamond-like carbon coating is 3% -38%; the H atoms on the solid phase surface of the diamond-like coating and the H atoms in the lubricating oil layer are used for repulsive interaction, so that the distribution of lubricating oil and the physical and chemical adsorption action of the lubricating oil on the solid phase surface of the diamond-like coating are influenced, in addition, the passivation action of H element on a friction interface is improved, the antifriction lubricating performance between two or more substrates with diamond-like coatings on the surfaces is also improved, meanwhile, the extrusion action of excessive hydrogenation on the solid phase surface of the diamond-like coating on the lubricating oil is prevented, and the friction resistance between the substrates is increased;
the preparation method of the ultra-low friction solid-liquid composite lubricating coating comprises the following steps:
a, etching and cleaning the surface of a substrate needing to prepare the composite lubricating coating by adopting an ion source and Ar gas as working gas sources so as to remove impurities on the surface of the substrate;
b, performing composite hydrogenation modification post-treatment by using magnetron sputtering to prepare a diamond-like coating with hydrogenated surface on the surface of the substrate; the specific process is as follows: firstly, starting a magnetron sputtering source, selecting high-purity graphite as a sputtering target material, introducing argon into the magnetron sputtering source, preparing a non-hydrogen diamond-like solid phase, then, switching off the magnetron sputtering source, switching on an ion source, and using H 2 For working gas source, the surface of non-hydrogen diamond-like solid phase is hydrogenated and modified by changing H 2 And controlling the atomic percentage content of H element on the surface of the prepared diamond-like solid phase, thereby preparing the surface hydrogenated diamond-like coating on the substrate.
2. The ultra-low friction solid-liquid composite lubricating coating according to claim 1, characterized in that: the matrix material of the matrix provided with the diamond-like carbon coating comprises a hard alloy material, a steel material, an aluminum alloy material, a magnesium alloy material and a titanium alloy material.
3. The ultra-low friction solid-liquid composite lubricating coating according to claim 1, characterized in that: the lubricating oil used in the lubricating oil layer comprises polyolefin, synthetic ester, polyalkyl ether, polysiloxane, alkylated aromatic/cyclic hydrocarbon and perfluoropolyether, and the liquid phase thickness of the lubricating oil layer is 0-100 nm.
4. The ultra-low friction solid-liquid composite lubricating coating according to claim 1, characterized in that: the diamond-like layer disposed on the substrate being of a general sp 2 、sp 3 The amorphous carbon material composed of the hybridized structure only contains C, H two constituent elements on the solid phase surface of the diamond-like carbon coating; the thickness of the diamond-like carbon layer arranged on the substrate is 0.1-4 mu m.
5. The ultra-low friction solid-liquid composite lubricating coating according to claim 1, characterized in that: the ion source operating current used in step a is 0.2A, the operating power is 200-350W, and the negative bias to the substrate is 100V.
6. The ultra-low friction solid-liquid composite lubricating coating according to claim 1, characterized in that: in step b, the negative bias voltage to the substrate is 50 to 150V.
7. The ultra-low friction solid-liquid composite lubricating coating according to claim 1, characterized in that: in the step b, in the magnetron sputtering deposition method for the substrate, the power of the magnetron sputtering target is 0.9-1.6 KW, and the working current is 1.5-3A.
8. The ultra-low friction solid-liquid composite lubricating coating according to claim 1, characterized in that: in the hydrogenation modification post-treatment method of the step b, the temperature of the hydrogenation surface modification treatment is controlled below 600K, H 2 The flow rate is 4.5-42 sccm.
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