CN111455386A - Ultra-smooth tungsten disulfide/hydrogen-containing carbon film and preparation method thereof - Google Patents
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- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
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- 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
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- 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
- C23C16/44—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 method of coating
- C23C16/50—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 method of coating using electric discharges
Abstract
The invention discloses an ultra-smooth tungsten disulfide/hydrogen-containing carbon film, which is characterized in that a double-layer film system is constructed on the surface of a substrate, and the double-layer film system comprises the hydrogen-containing carbon film attached to the surface of the substrate and WS attached to the surface of the carbon film2A spherical film. The invention relates to a carbon film prepared by a plasma vapor deposition method and WS prepared by a high-power pulse magnetron sputtering technology2The film ball forms a double-layer film system of hydrogen-containing carbon film-tungsten disulfide, under the action of frictional heat in the friction process, the tungsten disulfide catalyzes the hydrogen-containing diamond-like carbon film to generate two-dimensional graphene in situ, and the two-dimensional graphene is introducedAnd heterogeneous contact between the two is adopted to form multiphase interface non-degree contact so as to realize the ultra-smooth structure, thereby realizing the ultra-smooth structure under the atmosphere and argon atmosphere high-load environment on the macro scale.
Description
Technical Field
The invention relates to preparation of a composite hydrogen-carbon-containing film, in particular to an ultra-smooth tungsten disulfide/hydrogen-carbon-containing film and a preparation method thereof, belonging to the technical field of solid ultra-smoothness and tribology.
Background
In recent years, with the development of engineering technology, the working conditions of equipment operation are more and more complex and diversified, and higher requirements are put forward on low energy consumption, high reliability and long service life of moving parts. Especially, in the non-oil lubrication kinematic pair interface, how to reduce the adhesive wear and high temperature caused by high friction, even the equipment halt caused by friction fusion welding, and the like seriously influences the high-reliability and long-life operation of major engineering mechanical equipment.
The friction coefficient of the super-slip is in a state of 0.001, and the friction wear of the kinematic pair interface is expected to be reduced through the engineering application of the super-slip, so that the energy consumption is reduced, and the high reliability, long service life and stable operation of the key kinematic pair of the engineering mechanical equipment can be ensured. Among the solid lubricating materials, diamond-like carbon films, including non-hydrogen tetrahedral carbon films, hydrogen-containing tetrahedral carbon films, amorphous hydrogen-containing carbon films, have the lowest coefficient of friction among all film materials that can be engineered for use. Wherein, the hydrogen-containing carbon film has a low friction coefficient of about 0.05. At present, reports about ultra-smoothness are concentrated on the surface of a microscopic two-dimensional layered material, and engineering application is difficult to realize. Although it has been reported that the graphene can be introduced into the working interface to achieve large-scale ultra-smoothness, it is still a challenge how to prepare uniform two-dimensional layered materials on the complex surface of mechanical parts.
Disclosure of Invention
The invention aims to provide an ultra-smooth composite tungsten disulfide/hydrogen-containing carbon film and a preparation method thereof.
The invention discloses an ultra-smooth tungsten disulfide/hydrogen-containing carbon film, which is characterized in that: on a substrateConstructing a double-layer film system on the surface, wherein the double-layer film system comprises a hydrogen-containing carbon film deposited on the surface of a substrate and WS deposited on the surface of the carbon film2A film.
The hydrogen content of the hydrogen-containing carbon film is 10-30%, and the thickness of the hydrogen-containing carbon film is about 1 micron; the thickness of the tungsten disulfide film is less than 200 nm.
The preparation method of the ultra-smooth tungsten disulfide/hydrogen-containing carbon film comprises the steps of placing a substrate material into a film coating vacuum chamber after ultrasonic cleaning, vacuumizing to below 0.001 Pa, and preparing the hydrogen-containing carbon film by utilizing hollow cathode plasma or anode layer ion source auxiliary plasma; preparing WS by high-power pulse magnetron sputtering technology2A film.
The method for preparing the hydrogen-carbon-containing film by adopting the hollow cathode plasma comprises the following specific steps:
(1) introducing argon gas of 2Pa, carrying out hollow cathode current of 300-400A, carrying out bias voltage of 800V and cleaning for 30 minutes at the duty ratio, and further removing pollutants on the surface of the workpiece;
(2) replacing argon with 5 percent silane mixed gas of 2Pa, carrying out hollow cathode current 300A, bias voltage 200-400V and duty ratio 80 percent, and depositing a silicon bonding layer for 30 minutes;
(3) gradually introducing methane within 30 minutes until the ratio of the methane to the 5 percent silane gas mixture is 1:1, and keeping for 20 minutes;
(4) closing 5% silane mixed gas, introducing argon with the same amount, and controlling the ratio of methane to hydrogen to be 2:1-1: 2; depositing for 90 minutes; the obtained diamond-like carbon film has hydrogen content of 10-30%.
The method adopts an anode layer ion source to assist in preparing the hydrogen-carbon film, and comprises the following specific steps:
(1) 3Pa argon is introduced, the anode layer ion source voltage is 1500-2000V, the bias voltage is 800V, the duty ratio is 60 percent, and the cleaning is carried out for 30 minutes to further remove the pollutants on the surface of the workpiece;
(2) replacing argon with 5% silane gas mixture of 2Pa, anode layer ion source voltage of 1000-1200V, bias voltage of 200-400V, duty ratio of 60%, depositing a silicon bonding layer for 40 minutes;
(3) gradually introducing methane within 30 minutes until the ratio of the methane to the 5 percent silane mixed gas is 1:1, and keeping for 20 minutes;
(4) closing 5% silane mixed gas, introducing argon with the same amount, and controlling the ratio of methane to hydrogen to be 2:1-1: 2; the ion source voltage of the anode layer is 800-1000V, and the deposition is carried out for 90 minutes; the obtained diamond-like carbon film has hydrogen content of 10-30%.
Magnetron sputtering WS using high power pulses2: sputtering target using WS2The target was biased at 200V for a deposition time of 40 minutes under the conditions of an argon atmosphere, a gas pressure of 0.5 to 1Pa, a sputtering target voltage of 800V, a pulse wavelength of 1000 microseconds, and a pulse period of 2000 microseconds.
Second, friction performance of tungsten disulfide/hydrogen-containing carbon film
1. Friction performance in dry atmospheric environment
Cleaning and drying the surface of the prepared carbon film, fixing the carbon film on a steel sheet, and sputtering the obtained WS2And performing CSM friction test on the coated ball and the carbon film. Setting experiment parameters: the load is 3N, the frequency is 5Hz, the amplitude is 5mm, the air atmosphere is adopted, the rubbing time is 30min, and the room temperature rubbing is carried out. And introducing dry air, and controlling the air introduction rate to gradually reduce the friction humidity from 45% to 5% at a constant speed to obtain a CSM friction curve.
FIG. 2 is a graph of the ultra-smooth friction coefficient of the tungsten disulfide/hydrogen-containing carbon film prepared by the present invention in an atmospheric environment. As can be seen, the coefficient of friction using the friction partner system of the present invention is below 0.01, and as low as 0.002.
2. Friction performance under inert atmosphere
Cleaning and drying the surface of the prepared carbon film, fixing the carbon film on a steel sheet, and sputtering the obtained WS2And performing CSM friction test on the coated ball and the carbon film. Setting experiment parameters: the load is within the range of 3-7N, the frequency is 5Hz, the amplitude is 5mm, the friction time is 30min under the argon atmosphere, and the friction is carried out at room temperature. Argon was bubbled through to obtain a CSM friction curve.
FIG. 3 is a graph of the ultra-smooth friction coefficient of the tungsten disulfide/hydrogen-containing carbon film prepared by the present invention in an argon environment. As can be seen from the figure, the friction coefficient is about 0.002 at 5N, and the macroscopic ultra-smoothness under the argon high-load environment is realized.
Compared with the prior art, the invention has the following advantages:
1. the invention relates to a carbon film prepared by a plasma vapor deposition method and WS prepared by a high-power pulse magnetron sputtering technology2The film ball forms a double-layer film system of a hydrogen-containing carbon film-tungsten disulfide, under the action of frictional heat in the friction process, the tungsten disulfide catalyzes a hydrogen-containing diamond-like carbon film to generate two-dimensional graphene in situ, and heterogeneous contact between the two films forms multiphase interface non-metric contact to realize ultra-smooth structure, so that ultra-smooth in the atmosphere and argon atmosphere high-load environment on a macroscopic scale is realized;
2. the invention adopts the high-power pulse magnetron sputtering technology to prepare WS2The high-power pulse technology is different from the traditional magnetron sputtering, and the released energy is 100-100W/cm2(conventional magnetron sputtering releases energy of 10W/cm in a single pulse2) The air-space ratio reaches 30%, and the instantaneously released energy is 50-100 times of that of the direct current pulse; the micro-pulse mode can emit dozens or even hundreds of pulse waves in one period to form group waves, the pulse width is 1000 microseconds or even higher, and the prepared WS2The film ball has higher order;
3. the method can get rid of the limitation of the surface appearance of the complex parts and realize the uniform preparation of large-area and complex surfaces, so that the good lubricating property of the hydrogen-containing carbon film can be upgraded to be ultra-smooth, the wear resistance is better, the lubricating property under the harsh working condition is obviously improved, and a reliable choice is provided for the operation of mechanical parts under the harsh working condition.
Drawings
Figure 1 is a block diagram of a tungsten disulfide/hydrogen containing carbon film in accordance with the present invention.
FIG. 2 is a graph of the ultra-slip coefficient of friction of the tungsten disulfide/hydrogen-containing carbon film of the present invention in an atmospheric environment.
FIG. 3 is a graph of the ultra-slip coefficient of friction of the tungsten disulfide/hydrogen-containing carbon film of the present invention under argon.
Detailed Description
The preparation and tribological properties of the tungsten disulfide/hydrogen containing carbon film of the present invention are further illustrated by the following specific examples.
Example 1
(1) Ultrasonically cleaning a substrate material (which can be bearing steel, gear steel and the like), removing rusty spots and dirt, and inspecting the surface of a plated part after cleaning to ensure that no rusty spots or defects exist; putting the film into a vacuum film coating chamber, vacuumizing the chamber to be below 0.001 Pa, and starting film coating;
(2) the method for preparing the hydrogen-carbon-containing film by adopting the hollow cathode plasma comprises the following specific steps:
a. introducing argon gas of 2Pa, carrying out hollow cathode current of 300-400A, carrying out bias voltage of 800V and cleaning for 30 minutes at the duty ratio, and further removing pollutants on the surface of the workpiece;
b. replacing argon with 5 percent silane mixed gas of 2Pa, carrying out hollow cathode current 300A, bias voltage 200-400V and duty ratio 80 percent, and depositing a silicon bonding layer for 30 minutes;
c, gradually introducing methane within 30 minutes until the ratio of the methane to the 5 percent silane mixed gas is 1:1, and keeping for 20 minutes;
d. closing 5% silane mixed gas, introducing argon gas with the same amount, controlling the ratio of methane to hydrogen gas to be 2:1-1:2, and depositing for 90 minutes; a hydrogen content of 10-30% is obtained, and the thickness of the carbon film is about 1 micron.
(3) Magnetron sputtering WS using high power pulses2: turning off ion source, turning off methane and hydrogen, and turning on high-power pulse magnetron sputtering WS2: sputtering target using WS2And the target is biased at 200V under the conditions of argon atmosphere, air pressure of 0.5-1Pa, sputtering target voltage of 800V, pulse wavelength of 1000 microseconds and pulse period of 2000 microseconds, and the deposition time is 40 minutes. Obtaining the tungsten disulfide/hydrogen-containing carbon film, wherein the thickness of the tungsten disulfide film is less than 200 nm.
The tungsten disulfide/hydrogen-containing carbon film is loaded with 7N under the air condition, and the obtained friction coefficient is 0.003.
Example 2
(1) Ultrasonically cleaning a substrate material (which can be bearing steel, gear steel and the like), removing rusty spots and dirt, and inspecting the surface of a plated part after cleaning to ensure that no rusty spots or defects exist; putting the film into a vacuum film coating chamber, vacuumizing the chamber to be below 0.001 Pa, and starting film coating;
(2) the method adopts an anode layer ion source to assist in preparing the hydrogen-carbon film, and comprises the following specific steps:
a. 3Pa argon is introduced, the anode layer ion source voltage is 1500-2000V, the bias voltage is 800V, the duty ratio is 60 percent, and the cleaning is carried out for 30 minutes to further remove the pollutants on the surface of the workpiece;
b. replacing argon with 5% silane gas mixture of 2Pa, anode layer ion source voltage of 1000-1200V, bias voltage of 200-400V, duty ratio of 60%, depositing a silicon bonding layer for 40 minutes;
c, gradually introducing methane within 30 minutes until the ratio of the methane to the 5 percent silane mixed gas is 1:1, and keeping for 20 minutes;
d. closing 5% silane mixed gas, introducing argon with the same amount, and controlling the ratio of methane to hydrogen to be 2:1-1: 2; the ion source voltage of the anode layer is 800-1000V, and the deposition is carried out for 90 minutes; obtaining a carbon film with hydrogen content of 10-30%; the carbon film had a thickness of about 1 micron.
(3) Magnetron sputtering WS using high power pulses2: turning off ion source, turning off methane and hydrogen, and turning on high-power pulse magnetron sputtering WS2: sputtering target using WS2And (3) biasing the target at 200V under the conditions of argon atmosphere, air pressure of 0.5-1Pa, sputtering target voltage of 800V, pulse wavelength of 1000 microseconds and pulse period of 2000 microseconds, and depositing for 40 minutes to obtain the ultra-smooth composite tungsten disulfide/hydrogen-containing carbon film, wherein the thickness of the tungsten disulfide film is less than 200 nm.
The tungsten disulfide/hydrogen-containing carbon film is loaded with 5N under the condition of argon, and the obtained friction coefficient is 0.002.
Claims (7)
1. An ultra-smooth tungsten disulfide/hydrogen-containing carbon film is characterized in that: constructing a double-layer film system on the surface of a substrate, wherein the double-layer film system comprises a hydrogen-containing carbon film deposited on the surface of the substrate and WS deposited on the surface of the carbon film2A film.
2. The ultra-smooth tungsten disulfide/hydrogen-containing carbon film of claim 1, wherein: the hydrogen content of the hydrogen-carbon film is 10-30%.
3. The ultra-smooth tungsten disulfide/hydrogen-containing carbon film of claim 1, wherein: the thickness of the hydrogen-containing carbon film is less than 1 micron; the thickness of the tungsten disulfide film is less than 200 nm.
4. The method of claim 1, wherein the ultra-smooth tungsten disulfide/hydrogen-containing carbon film is prepared by cleaning a substrate with ultrasound, placing the substrate in a vacuum chamber, vacuumizing to below 0.001 Pa, and preparing a hydrogen-containing carbon film by using a hollow cathode plasma or an anode layer ion source assisted plasma; preparing WS by high-power pulse magnetron sputtering technology2A film.
5. The method of claim 4, wherein the ultra-smooth tungsten disulfide/hydrogen-containing carbon film is prepared by: the method for preparing the hydrogen-carbon-containing film by adopting the hollow cathode plasma comprises the following steps:
(1) introducing argon gas of 2Pa, carrying out hollow cathode current of 300-400A, carrying out bias voltage of 800V and cleaning for 30 minutes at the duty ratio, and further removing pollutants on the surface of the workpiece;
(2) replacing argon with 5 percent silane mixed gas of 2Pa, carrying out hollow cathode current 300A, bias voltage 200-400V and duty ratio 80 percent, and depositing a silicon bonding layer for 30 minutes;
(3) gradually introducing methane within 30 minutes until the ratio of the methane to the 5 percent silane gas mixture is 1:1, and keeping for 20 minutes;
(4) closing 5% silane mixed gas, introducing argon with the same amount, and controlling the ratio of methane to hydrogen to be 2:1-1: 2; depositing for 90 minutes; the obtained diamond-like carbon film has hydrogen content of 10-30%.
6. The method of claim 4, wherein the ultra-smooth tungsten disulfide/hydrogen-containing carbon film is prepared by: the method for preparing the hydrogen-carbon film by adopting the anode layer ion source assistance comprises the following steps:
(1) 3Pa argon is introduced, the anode layer ion source voltage is 1500-2000V, the bias voltage is 800V, the duty ratio is 60 percent, and the cleaning is carried out for 30 minutes to further remove the pollutants on the surface of the workpiece;
(2) replacing argon with 5% silane gas mixture of 2Pa, anode layer ion source voltage of 1000-1200V, bias voltage of 200-400V, duty ratio of 60%, depositing a silicon bonding layer for 40 minutes;
(3) gradually introducing methane within 30 minutes until the ratio of the methane to the 5 percent silane mixed gas is 1:1, and keeping for 20 minutes;
(4) closing 5% silane mixed gas, introducing argon with the same amount, and controlling the ratio of methane to hydrogen to be 2:1-1: 2; the ion source voltage of the anode layer is 800-1000V, and the deposition is carried out for 90 minutes; the obtained diamond-like carbon film has hydrogen content of 10-30%.
7. The method of claim 4, wherein the ultra-smooth tungsten disulfide/hydrogen-containing carbon film is prepared by: magnetron sputtering WS using high power pulses2: sputtering target using WS2The target was biased at 200V for a deposition time of 40 minutes under the conditions of an argon atmosphere, a gas pressure of 0.5 to 1Pa, a sputtering target voltage of 800V, a pulse wavelength of 1000 microseconds, and a pulse period of 2000 microseconds.
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Cited By (5)
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| CN111876753A (en) * | 2020-08-04 | 2020-11-03 | 中国科学院兰州化学物理研究所 | Method for realizing ultra-smooth macroscopic view by forming auxiliary system by hydrogen-containing carbon film and molybdenum disulfide |
| CN111876754A (en) * | 2020-08-04 | 2020-11-03 | 中国科学院兰州化学物理研究所 | Method for realizing macroscopic super-lubricity by matching nano metal coated steel ball and hydrogen-carbon-containing film |
| CN112210417A (en) * | 2020-10-21 | 2021-01-12 | 中国科学院兰州化学物理研究所 | Friction catalysis design method for realizing ultralow friction of carbon film |
| CN113215525A (en) * | 2021-05-18 | 2021-08-06 | 中国科学院兰州化学物理研究所 | Rubber surface ultra-low friction multilayer composite carbon-based lubricating coating and construction method thereof |
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| CN111876754A (en) * | 2020-08-04 | 2020-11-03 | 中国科学院兰州化学物理研究所 | Method for realizing macroscopic super-lubricity by matching nano metal coated steel ball and hydrogen-carbon-containing film |
| JP2022029418A (en) * | 2020-08-04 | 2022-02-17 | 中国科学院蘭州化学物理研究所 | Method for achieving super lubrication in macroscopic scale by forming pair system with hydrogen-containing carbon film and molybdenum disulfide |
| JP7152561B2 (en) | 2020-08-04 | 2022-10-12 | 中国科学院蘭州化学物理研究所 | A Method for Realizing Super Lubrication on a Macroscopic Scale by Forming a Pair System with a Hydrogen-Containing Carbon Film and Molybdenum Disulfide |
| US11927217B2 (en) | 2020-08-04 | 2024-03-12 | Lanzhou Institute Of Chemical Physics, Chinese Academy Of Sciences | Method for realizing macroscopic super-lubrication by a matching pair of nano metal-coated steel balls and hydrogen-containing carbon films |
| CN112210417A (en) * | 2020-10-21 | 2021-01-12 | 中国科学院兰州化学物理研究所 | Friction catalysis design method for realizing ultralow friction of carbon film |
| CN113215525A (en) * | 2021-05-18 | 2021-08-06 | 中国科学院兰州化学物理研究所 | Rubber surface ultra-low friction multilayer composite carbon-based lubricating coating and construction method thereof |
| CN114142763A (en) * | 2021-12-03 | 2022-03-04 | 中国科学院兰州化学物理研究所 | Nano friction generator |
| CN114142763B (en) * | 2021-12-03 | 2024-03-19 | 中国科学院兰州化学物理研究所 | Nanometer friction generator |
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