CN114196913A - A kind of ultra-low friction solid-liquid composite lubricating coating and preparation method thereof - Google Patents
A kind of ultra-low friction solid-liquid composite lubricating coating and preparation method thereof Download PDFInfo
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- 239000011248 coating agent Substances 0.000 title claims abstract description 95
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- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 239000007788 liquid Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- 239000000758 substrate Substances 0.000 claims abstract description 74
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- 238000012986 modification Methods 0.000 claims description 20
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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
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- 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
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- 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
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- 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
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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
- C23C14/22—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
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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
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
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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 two or more substrates which have mutual friction working conditions, the diamond-like coating is arranged on a mutual friction surface of the substrates, and a lubricating oil layer serving as an intermediate liquid phase is arranged between the two or more substrates which have mutual friction working conditions; the diamond-like coating is only hydrogenated on the surface, and the hydrogenated surface contains 3 to 38 percent of H element atoms. The diamond 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 composite lubricating coating material has excellent comprehensive performance, long service life and high reliability.
Description
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 which is suitable for industrial and mining enterprises and a preparation method thereof, belonging to the technical field of material surface coating.
Background
In recent years, the high-technology industries such as oceans, aviation, automobiles, micro-electro-mechanical systems and the like are rapidly developed, mechanical key moving parts face serious friction and wear problems, especially under double pressure of energy and environment, the traditional lubricating grease material or the solid lubricating coating with a single component and a single structure is difficult to meet the requirements of wear resistance, lubrication and bearing performance under the conditions of complex, variable and harsh working conditions (temperature, humidity, pressure, load, material and the like), and the research and development of a new generation of high-performance lubricating material and lubricating technology with the characteristics of ultralow friction, high bearing, long service life, good environmental adaptability and the like are urgently needed, so that the key way of prolonging the service life of the parts, realizing reliable operation, saving energy and reducing consumption is provided.
Diamond-like carbon (DLC) is mainly composed of sp3Bonds (diamond phase) and sp2The 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 the most ideal surface modified solid lubricating material of key moving parts, has become one of the hot spots which are paid attention to in the twenty-first century, can be successfully obtained under the environment-friendly, dry and low-temperature physical/chemical vapor deposition technology, and meets the national important strategic requirements on energy conservation, consumption reduction and emission reduction.
However, in the field of DLC basic research and engineering applications, there are major problems as follows: large residual stress, poor film-substrate bonding force, and weak bonding with soft metal; secondly, the lubricating performance is greatly influenced by the environmental atmosphere (temperature, humidity, pressure, medium and the like); the lubricating effect is not as good as that of fluid lubrication, and the friction coefficient is almost higher than that of grease lubrication by several times to dozens of times; self-consumption type lubrication, and the service life has a certain limit, thereby greatly limiting the wide application and industrialization promotion of the DLC solid lubricating material.
The design and control of the composite structure of the DLC material and the synergistic lubrication technology compounded with lubricating oil, additives and the like are effective ways for solving the key technology and application bottleneck, prolonging the service life of parts, realizing reliable operation, saving energy and reducing consumption. However, the friction and the wear are closely related to the surface/interface structure of the material, and the combination of coating materials with different structures and the interface optimization generate different surface/interface structures, thereby further influencing the friction characteristics of the coating and the basic physicochemical characteristics of the lubricating oil, additives on the surface, such as adsorption, wetting and the like.
Therefore, how to realize the synergistic lubrication of DLC and lubricating oil and develop a high-performance solid-liquid composite lubricating material and technology through the surface/interface structure design and regulation of DLC solid phase is one of important research contents in the field of tribology and also is a very active field in 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 arranged on a friction surface 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 coating is only subjected to surface hydrogenation, and the percentage content of H element atoms contained on the surface of the solid phase of the diamond-like coating is 3-38%; the method utilizes the repulsion action between the H atoms on the surface of the solid phase of the diamond-like coating and the H atoms in the lubricating oil layer to influence the distribution of the lubricating oil and the physical and chemical adsorption action of the lubricating oil on the surface of the solid phase of the diamond-like coating, and in addition, the passivation action of the H elements on a friction interface also improves the antifriction lubricating performance between two or more substrates with the diamond-like coating on the surfaces, and simultaneously prevents the excessive hydrogenation on the surface of the solid phase of the diamond-like coating from extruding the lubricating oil, and on the contrary, increases the friction resistance between the substrates.
The base body provided with the diamond-like 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 for the lubricating oil layer comprises polyolefin, synthetic ester, polyalkyl ether, polysiloxane, alkylated aromatic/cyclic hydrocarbon and perfluoropolyether, and the thickness of a liquid phase of the lubricating oil layer is 0-100 nm.
The diamond-like carbon layer arranged on the substrate is sp-like2、sp3Amorphous carbon material composed of hybrid structure, wherein only the surface of the diamond-like coating solid phase contains C, H two constituent elements; the thickness of the diamond-like carbon layer arranged on the substrate is 0.1-4 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 using an ion source and Ar gas as a working gas source to remove impurities on the surface of the substrate;
b, performing magnetron sputtering composite hydrogenation modification post-treatment to prepare a diamond-like coating with a hydrogenated surface on the surface of the substrate; the specific process is as follows: firstly, opening a magnetron sputtering source, selecting high-purity graphite as a sputtering target material, introducing argon into the magnetron sputtering source, prefabricating a hydrogen-free diamond solid phase, then closing the magnetron sputtering source, opening an ion source, and taking H as2The surface of the hydrogen-free diamond solid phase is subjected to hydrogenation modification treatment by changing H for serving as a working gas source2Controlling the flow rate, and controlling the atomic percentage content of the H element on the surface of the prefabricated diamond-like solid phase, so as to prepare a diamond-like coating with a hydrogenated surface on the substrate;
further, the working current of the ion source used in the step a is 0.2A, the working power is 200-350W, and the negative bias voltage for the substrate is 100V.
Further, in the step b, the negative bias voltage for the substrate is 50-150V.
Further, in the step b, in the method for carrying out magnetron sputtering deposition on the substrate, the magnetron sputtering target power is 0.9-1.6 KW, and the working current is 1.5-3A.
Further, in the method for post-treatment of hydrogenation modification in step b, the temperature of the hydrogenation surface modification treatment is controlled to be 600K or less, H2The flow rate is 4.5 to 42 sccm.
Has the advantages that:
firstly, 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 resistance, corrosion resistance, bearing and the like, and the fluid lubrication action of the lubricating oil is added, so that the self consumption of the diamond-like solid phase can be obviously reduced, and the friction performance can be synergistically improved; secondly, in the composite lubricating coating, the atomic percentage of the H element on the surface of the self-prepared diamond-like solid phase is 3-38%, because the repulsion action exists between the H atoms on the surface of the diamond-like solid phase and the H atoms in the lubricating oil, the distribution of the lubricating oil and the physical and chemical adsorption action of the lubricating oil on the surface of the diamond-like solid phase are influenced, and the passivation action of H on a friction interface is added, so that the friction-reducing lubricating performance is optimal (the friction coefficient is between 0 and 0.01), and the phenomenon that the lubricating oil is extruded by excessive hydrogenation on the surface of the diamond-like solid phase to increase the friction resistance can be avoided. Third, in the composite lubricating coating, the diamond-like solid phase contains only C, H two constituent elements, thereby avoiding the generation of frictional wear induced by solid phase corrosion during the rubbing process. Fourthly, the composite lubricating coating has a wide range of applicable substrates, including hard alloy, various steels, aluminum alloy, magnesium alloy, titanium alloy and the like; the friction stability of the matrix used under complicated and changeable working conditions such as rich, poor and oil-free conditions is excellent, and the service life and the reliability are prolonged.
The preparation method of the solid-liquid composite lubricating coating has the following advantages:
firstly, the magnetron sputtering composite hydrogenation modification post-treatment method is adopted for deposition, the large-area uniform and low-temperature deposition of the surface-hydrogenated diamond-like solid phase can be realized, the operation is simple and easy to control, and the industrialized application is facilitated. Second, the magnetron sputtering is combined with the post-hydrogenation modificationIn the method, the temperature of surface modification treatment is controlled below 600K, the intrinsic mechanical property of the diamond-like solid phase is not damaged while surface hydrogenation is carried out, and the comprehensive performance is optimal. Thirdly, using H2As a working air source, the accurate regulation and control of different H element contents on the surface of the diamond-like solid phase can be realized by regulating the flow of the air source.
Drawings
FIG. 1 is a graph comparing friction coefficients of samples of the solid-liquid composite lubricating coatings obtained in example 1 and comparative examples 1-2;
FIG. 2 is a graph comparing the friction coefficients of samples of the solid-liquid composite lubricating coatings obtained in example 2 and comparative examples 1-2;
FIG. 3 is a graph comparing the friction coefficients of samples of the solid-liquid composite lubricating coatings obtained 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 a self-matched upper and lower solid phase, 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, lubrication resistance, corrosion resistance, bearing and the like, and the fluid lubrication behavior of lubricating oil is added, so that the friction performance is improved synergistically. Specifically, the ultralow-friction solid-liquid composite lubricating coating is a diamond-like coating arranged on two or more substrates which have mutual friction working conditions, specifically the diamond-like coating is arranged on the friction contact surface of the substrates which have mutual friction, and a lubricating oil layer serving as an intermediate liquid phase is arranged between the two or more substrates which have mutual friction working conditions; wherein the diamond-like coating is only subjected to surface hydrogenation, and the percentage content of H element atoms contained on the surface of the solid phase of the diamond-like coating is 3-38%; the friction reducing and lubricating performance is optimized by utilizing the repulsion action between the H atoms on the surface of the diamond-like coating solid phase and the H atoms in the lubricating oil layer to influence the distribution of the lubricating oil and the physical and chemical adsorption action of the lubricating oil on the surface of the diamond-like coating solid phase, and in addition, the passivation action of the H element on a friction interface. The friction-reducing lubricating performance between two or more substrates with the diamond-like carbon layers on the surfaces is also improved, and the excessive hydrogenation of the surfaces of the diamond-like carbon coating solid phases is prevented from generating extrusion effect on lubricating oil, but the frictional resistance between the substrates is increased.
The friction coefficient of the coating is 0-0.01.
The substrate of the coating is hard alloy, various steels, aluminum alloy, magnesium alloy, titanium alloy and the like.
The liquid phase of the coating is polyolefin, synthetic ester, polyalkyl ether, polysiloxane, alkylated aromatic/cyclic hydrocarbon, perfluoropolyether, etc.
The liquid phase thickness of the coating is 0-100 nm.
The diamond-like solid phase of the coating is sp-like2、sp3The 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:
firstly, 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 resistance, corrosion resistance, bearing and the like, and the fluid lubrication behavior of the lubricating oil is added, so that the self consumption of the diamond-like solid phase can be obviously reduced, and the friction performance can be synergistically improved. Secondly, in the composite lubricating coating, the atomic percentage of the H element on the surface of the self-prepared diamond-like solid phase is 3-38% respectively, because the repulsion action exists between the H atoms on the surface of the diamond-like solid phase and the H atoms in the lubricating oil, the distribution of the lubricating oil and the physical and chemical adsorption action of the lubricating oil on the surface of the diamond-like solid phase are influenced, and the passivation action of H on a friction interface is added, so that the friction-reducing lubricating performance is optimal (the friction coefficient is between 0-0.01), and the phenomenon that the lubricating oil is extruded by excessive hydrogenation on the surface of the diamond-like solid phase to increase the friction resistance can be avoided. Third, in the composite lubricating coating, the diamond-like solid phase contains only C, H two constituent elements, thereby avoiding the generation of frictional wear induced by solid phase corrosion during the rubbing process. Fourthly, the composite lubricating coating has a wide range of applicable substrates, including hard alloy, various steels, aluminum alloy, magnesium alloy, titanium alloy and the like; the friction stability of the matrix used under complicated and changeable working conditions such as rich, poor and oil-free conditions is excellent, and the service life and the reliability are prolonged.
The invention also provides a preparation method of the solid-liquid composite lubricating coating, and the preparation method of the diamond-like solid phase of the coating 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) magnetron sputtering is adopted for composite hydrogenation modification post-treatment, and the diamond-like solid phase with hydrogenated surface is prepared.
In the step (1), the aim of etching and cleaning the substrate is to remove surface impurities on one hand and enlarge the surface of the substrate 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), the diamond-like solid phase is prepared by adopting a magnetron sputtering composite hydrogenation modification post-treatment method, 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, the hydrogen-free diamond-like carbon is prepared, then the magnetron sputtering source is closed, the ion source is opened, and H is used2Performing surface hydrogenation modification as a working gas source, and controlling the atomic percentage content of the H element on the surface of the solid phase by changing the hydrogen flow; the magnetron sputtering target has the power of 0.9-1.6 KW, the working current of 1.5-3A and the negative bias of a substrate of 50-150V; the temperature of the modification treatment of the hydrogenated surface is controlled below 600K, H2The flow rate is 4.5 to 42 sccm.
The preparation method of the solid-liquid composite lubricating coating has the following advantages:
firstly, adopting magnetron sputtering to compound the post-hydrogenation modificationThe physical method deposition can realize large-area uniform and low-temperature deposition of the surface-hydrogenated diamond-like solid phase, is simple and easy to control in operation, and is 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 property of the diamond-like solid phase is not damaged while the surface is hydrogenated, and the comprehensive performance is optimal. Thirdly, using H2The accurate regulation and control of different H element contents on the surface of the diamond-like solid phase is realized by regulating the flow of the gas source serving as a working gas source
The tough wear-resistant coating and the preparation method thereof of the invention are explained below with reference to specific examples:
example 1:
(1) placing the substrate subjected to ultrasonic cleaning on a workpiece bracket of a vacuum chamber;
(2) the air pressure of the vacuum chamber is adjusted to 2.7 multiplied by 10-3Pa, starting a linear ion source, introducing 40sccm argon gas into the linear ion source, setting the working current of the linear ion source to be 0.2A and the working power to be 280W, setting the negative bias of the substrate to be 100V, and cleaning and etching the substrate for 15 min;
(3) deposition of diamond-like solid phases on the surface of a substrate
Starting a magnetron sputtering source, and preparing a hydrogen-free diamond solid phase in advance: the magnetron sputtering source is a high-purity graphite target (the purity is not less than 99.99%), argon is introduced into the magnetron sputtering source, the gas flow is 50sccm, the magnetron sputtering target power is 1350W, the working current is 2.8A, the negative bias of the substrate is set to 50V, the working gas 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 introduced2The ion source is a working gas source, the gas flow is 30sccm, the ion source working current is 0.2A, and the working power is 250W; the substrate negative bias voltage is set to 50V; the heating temperature of the substrate is 400K.
(4) And opening the cavity when the temperature of the vacuum chamber is reduced to room temperature, and taking out the substrate, wherein the surface of the substrate is the surface hydrogenated diamond-like solid phase.
(5) The prepared diamond-like carbon 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 to a friction interface of the upper solid phase and the lower solid phase to form a solid-liquid composite lubricating coating.
In the prepared solid-liquid composite lubricating coating, 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 respectively 18.8% and 18.8%; the thickness of the polyolefin lubricating oil was 5 nm. The friction test showed that the coefficient of friction of the coating was 0.007 at a contact pressure of 5GPa, as shown in fig. 1.
Example 2:
(1) placing the substrate subjected to ultrasonic cleaning on a workpiece bracket of a vacuum chamber;
(2) the air pressure of the vacuum chamber is adjusted to 2.7 multiplied by 10-3Pa, starting a linear ion source, introducing 40sccm argon gas into the linear ion source, setting the working current of the linear ion source to be 0.2A and the working power to be 280W, setting the negative bias of the substrate to be 100V, and cleaning and etching the substrate for 15 min;
(3) deposition of diamond-like solid phases on the surface of a substrate
Starting a magnetron sputtering source, and preparing a hydrogen-free diamond solid phase in advance: the magnetron sputtering source is a high-purity graphite target (the purity is not less than 99.99%), argon is introduced into the magnetron sputtering source, the gas flow is 50sccm, the magnetron sputtering target power is 1350W, the working current is 2.8A, the negative bias of the substrate is set to 50V, the working gas 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 introduced2The ion source is a working gas source, the gas flow is 35sccm, the ion source working current is 0.2A, and the working power is 260W; the substrate negative bias voltage is set to 50V; the heating temperature of the substrate is 400K.
(4) And opening the cavity when the temperature of the vacuum chamber is reduced to room temperature, and taking out the substrate, wherein the surface of the substrate is the surface hydrogenated diamond-like solid phase.
(5) The diamond-like carbon prepared above serves 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)2The gas flow is 5sccm, and the prepared diamond-like carbon is used as an upper solid phase of the composite coating.
(7) Polyolefin is selected as lubricating oil and added to a friction interface consisting of an upper solid phase and a lower solid phase of the prepared diamond-like carbon to form a solid-liquid composite lubricating coating.
In the prepared solid-liquid composite lubricating coating, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are both 0.8 mu m, and the atomic percentage content of the surface H element is respectively 3.6 percent and 24.9 percent; the thickness of the polyolefin lubricating oil was 5 nm. The friction test shows that the friction coefficient of the coating is 0.003 under the contact pressure of 5GPa, as shown in figure 2.
Example 3:
(1) placing the substrate subjected to ultrasonic cleaning on a workpiece bracket of a vacuum chamber;
(2) the air pressure of the vacuum chamber is adjusted to 2.7 multiplied by 10-3Pa, starting a linear ion source, introducing 40sccm argon gas into the linear ion source, setting the working current of the linear ion source to be 0.2A and the working power to be 280W, setting the negative bias of the substrate to be 100V, and cleaning and etching the substrate for 15 min;
(3) deposition of diamond-like solid phases on the surface of a substrate
Starting a magnetron sputtering source, and preparing a hydrogen-free diamond solid phase in advance: the magnetron sputtering source is a high-purity graphite target (the purity is not less than 99.99%), argon is introduced into the magnetron sputtering source, the gas flow is 50sccm, the magnetron sputtering target power is 1350W, the working current is 2.8A, the negative bias of the substrate is set to 50V, the working gas 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 introduced2The ion source is a working gas source, the gas flow is 40sccm, the ion source working current is 0.2A, and the working power is 280W; the substrate negative bias voltage is set to 50V; the heating temperature of the substrate is 400K.
(4) And opening the cavity when the temperature of the vacuum chamber is reduced to room temperature, and taking out the substrate, wherein the surface of the substrate is the surface hydrogenated diamond-like solid phase.
(5) The diamond-like carbon prepared above serves 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)2The gas flow is 30sccm, and the prepared diamond-like carbon is used as an upper solid phase of the composite coating.
(7) Polyolefin is selected as lubricating oil and added to a friction interface consisting of an upper solid phase and a lower solid phase of the prepared diamond-like carbon to form a solid-liquid composite lubricating coating.
In the prepared solid-liquid composite lubricating coating, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are both 0.8 mu m, and the atomic percentage contents of surface H elements are respectively 18.8% and 34.1%; the thickness of the polyolefin lubricating oil was 5 nm. The friction test showed that the coefficient of friction 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 the above examples 1, 2, 3.
In this example, the preparation method of the solid-liquid composite lubricating coating is substantially the same as that in example 1, except that in step (3), after the hydrogen-free diamond solid phase is prepared in advance, the ion source is not started to perform surface hydrogenation modification treatment, and other process steps are the same as those in example 1.
In the prepared solid-liquid composite lubricating coating, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are both 0.8 mu m through test analysis, and the atomic percentage content of the surface H element is respectively 0% and 0%; the thickness of the polyolefin lubricating oil was 5 nm. The friction test shows that the friction coefficient of the coating at the contact pressure of 5GPa is 0.024, as shown in figures 1, 2 and 3.
Comparative example 2:
this example is a comparative example of the above examples 1, 2, 3.
In this example, the preparation method of the solid-liquid composite lubricating coating was substantially the same as in example 1, except that in step (3), the surface hydrogenation modification treatment was performed on the hydrogen-free diamond solid phase, and H was introduced2The gas flow rate was 45sccm, and the other process steps were the same as in example 1.
In the prepared solid-liquid composite lubricating coating, the thicknesses of the upper diamond-like solid phase and the lower diamond-like solid phase are both 0.8 mu m, and the atomic percentage contents of surface H elements are respectively 44.1% and 44.1%; the thickness of the polyolefin lubricating oil was 5 nm. Through a friction test, the friction coefficient of the coating at the contact pressure of 5GPa is 0.042, as shown in figures 1, 2 and 3.
Claims (9)
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