CN110965015A - CrN/MoS2 solid self-lubricating composite film - Google Patents

CrN/MoS2 solid self-lubricating composite film Download PDF

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CN110965015A
CN110965015A CN201811148943.3A CN201811148943A CN110965015A CN 110965015 A CN110965015 A CN 110965015A CN 201811148943 A CN201811148943 A CN 201811148943A CN 110965015 A CN110965015 A CN 110965015A
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张亮东
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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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
    • 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
    • C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding

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  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

A CrN/MoS2 solid self-lubricating composite membrane is based on the super-lubricating property of MoS2, and a composite plating and infiltration method is adopted for further reducing the dry friction resistance of a CrN-based composite membrane, namely a novel method for treating the CrMoN composite membrane by low-temperature ion sulfurization is adopted, and the CrN/MoS2 solid self-lubricating composite membrane with excellent tribology performance is synthesized in situ. After the CrMoN composite membrane is subjected to sulfurization treatment, a MoS2 lubricating phase is mainly synthesized, the thickness of a sulfurization layer is about 500nm, and the main phase structure comprises CrN, MoS2 and a small amount of MoN. Compared with the CrMoN composite membrane, the CrN/MoS2 solid self-lubricating composite membrane has the advantages of lower friction coefficient, smaller abrasion volume, better wear resistance and antifriction property.

Description

CrN/MoS2 solid self-lubricating composite film
Technical Field
The invention relates to a solid film material, in particular to a CrN/MoS2 solid self-lubricating composite film.
Background
The solid lubrication can meet some special working conditions which cannot be met by the fluid lubrication, such as high temperature, high load, ultralow temperature, ultrahigh vacuum, strong oxidation, strong radiation and the like. The solid lubricating film can form a transfer film on the surface of the mating material during friction, so that the friction is generated in the film, thereby reducing the friction and reducing the abrasion. The lubricating film can prevent the surfaces of the mating materials from directly contacting on one hand, and can reduce the shear strength of the contact thin layer on the other hand, thereby reducing the friction coefficient.
The research and development of the CrN-based composite membrane opens up a wide space for further improving the performance of the CrN film. In the aspect of reducing the friction coefficient of the CrN film, the research on the CrMoN composite film is mainly focused. Research shows that MoO can be formed on the friction surface by adding Mo element into CrN film3The self-lubricating phase is beneficial to reducing the friction coefficient of the film; but due to MoO3Moistening of the phasesThe sliding effect is limited, so that the friction coefficient of the CrMoN composite membrane is reduced to a limited extent. The MoS2 crystal has a hexagonal layered structure, and weak van-der-force exists among crystal faces, so that displacement is easy to occur. In addition, the MoS2 film is loose and porous, has strong oil storage capacity, can form a continuous and unbreakable lubricating oil film on the friction surface, and effectively hinders the direct contact between metals. Common methods for preparing the MoS2 film include plasma plating, organic bonding, sputtering deposition and the like.
Disclosure of Invention
The invention aims to improve the wear resistance of a stainless steel composite material and designs a CrN/MoS2 solid self-lubricating composite film.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the preparation raw materials of the CrN/MoS2 solid self-lubricating composite membrane comprise: reagents used for synthesis of nano MoS 2: sodium molybdate (A.R) (Shanghai colloid chemical plant). Hydroxylamine hydrochloride (A.R), thiourea (A.R) (standard technologies, ltd, Tianjin). Absolute ethanol (A.R) (national pharmaceutical group chemical Co., Ltd.).
The preparation method of the CrN/MoS2 solid self-lubricating composite membrane comprises the following steps: using a magnetron sputtering apparatus at N2Co-sputtering Cr target and Mo target in atmosphere to deposit CrMoN composite film in the thickness of 5-6 micron on the surface of stainless steel. The CrN/MoS2 solid self-lubricating composite membrane is prepared by using high-frequency pulse plasma diffusion equipment and taking sulfur vapor as a sulfur permeation source to carry out low-temperature (230 ℃) ion sulfur permeation treatment on the surface of the membrane for 2 hours.
The detection steps of the CrN/MoS2 solid self-lubricating composite membrane are as follows: and (3) observing the surface appearance and the grinding trace appearance of the film by using a Philips Quant200 type Scanning Electron Microscope (SEM), and analyzing the microstructure and the friction and wear mechanism of the composite film. The resolution is 3.5nm, the magnification is 200-120000 times, the accelerating voltage is 30kV, the maximum beam current is 2A, and meanwhile, a Genesis type energy spectrometer (EDS) is adopted to analyze the chemical components of the sulfurizing layer. The compound valence state of the CrN-based solid self-lubricating composite membrane is researched by using an ESCALB 250Xi type X-ray photoelectron spectrometer (XPS). Excitation source: al target, fine sweep width: 25 eV. And analyzing the component distribution of the cross section of the CrN-based solid self-lubricating composite membrane by using a PHI700 Auger electron energy spectrometer (AES). The fretting wear resistance of the film is tested by adopting a CETR UTM-2 type friction wear testing machine. The experimental conditions were: the motion mode is reciprocating type, room temperature air environment, and the mating part is a GCr15 steel ball with the diameter of 4.0 mm. The load range is 20-80N; the frequency range is 2-8 Hz; the temperature is 23-26 ℃. Friction environment: dry friction in the atmosphere or tank oil lubrication. And (3) testing a grinding mark profile curve of the surface of the sample by adopting a TR240 surface roughness meter, and calculating the wear volume of the film according to a wave trough on the curve.
The invention has the beneficial effects that:
the CrMoN composite membrane is successfully prepared by a magnetron sputtering technology, and low-temperature ion sulfurization treatment is carried out on the surface of the membrane by using high-frequency pulse plasma diffusion and permeation equipment, so that the CrN/MoS2 solid self-lubricating composite membrane containing a MoS2 lubricating phase is successfully prepared. 2 films are all compact and flat columnar crystal structures, and the grain sizes all reach the nanometer level; the CrN/MoS2 solid self-lubricating composite membrane embeds a layered MoS2 soft phase in a (Cr, Mo) N hard phase to form a novel concrete structural film. The thickness of the CrN/MoS2 solid self-lubricating composite film is about 500nm, the CrN/MoS2 solid self-lubricating composite film mainly comprises Cr, Mo, N and S4 elements, and a sulfurization product mainly comprises a MoS2 lubricating phase. The main phase structures of the CrN/MoS2 solid self-lubricating composite membrane are CrN, MoS2 and a small amount of MoN. Compared with the dry friction condition, the friction coefficient of the 2 films is obviously reduced under the oil lubrication condition, the fluctuation along with the change of the distance is relatively stable, and the abrasion volume is reduced by 1 order of magnitude compared with that under the dry friction condition. Abrasion volume value size: CrMoN is more than CrN/MoS2, which shows that the CrN/MoS2 solid self-lubricating composite membrane has higher sliding wear resistance. No matter under dry friction or oil lubrication condition, the CrN/MoS2 solid self-lubricating composite film is worn by abrasive particles, the wear degree is slight compared with that of the CrMoN composite film, and the synthetic MoS2 lubricating phase in the composite film enables the wear resistance and the friction reducing performance of the CrN/MoS2 solid self-lubricating composite film to be greatly improved. Under the condition of dry friction, the CrMoN composite membrane even has severe adhesive wear; under the condition of oil lubrication, the surface wear of the 2 films is greatly reduced. Therefore, the oil lubrication condition can effectively improve the wear resistance and the abrasion resistance of the film.
Detailed Description
Example 1:
the preparation raw materials of the CrN/MoS2 solid self-lubricating composite membrane comprise: reagents used for synthesis of nano MoS 2: sodium molybdate (A.R) (Shanghai colloid chemical plant). Hydroxylamine hydrochloride (A.R), thiourea (A.R) (standard technologies, ltd, Tianjin). Absolute ethanol (A.R) (national pharmaceutical group chemical Co., Ltd.). The preparation method of the CrN/MoS2 solid self-lubricating composite membrane comprises the following steps: using a magnetron sputtering apparatus at N2Co-sputtering Cr target and Mo target in atmosphere to deposit CrMoN composite film in the thickness of 5-6 micron on the surface of stainless steel. The CrN/MoS2 solid self-lubricating composite membrane is prepared by using high-frequency pulse plasma diffusion equipment and taking sulfur vapor as a sulfur permeation source to carry out low-temperature (230 ℃) ion sulfur permeation treatment on the surface of the membrane for 2 hours. The detection steps of the CrN/MoS2 solid self-lubricating composite membrane are as follows: and (3) observing the surface appearance and the grinding trace appearance of the film by using a Philips Quant200 type Scanning Electron Microscope (SEM), and analyzing the microstructure and the friction and wear mechanism of the composite film. The resolution is 3.5nm, the magnification is 200-120000 times, the accelerating voltage is 30kV, the maximum beam current is 2A, and meanwhile, a Genesis type energy spectrometer (EDS) is adopted to analyze the chemical components of the sulfurizing layer. The compound valence state of the CrN-based solid self-lubricating composite membrane is researched by using an ESCALB 250Xi type X-ray photoelectron spectrometer (XPS). Excitation source: al target, fine sweep width: 25 eV. And analyzing the component distribution of the cross section of the CrN-based solid self-lubricating composite membrane by using a PHI700 Auger electron energy spectrometer (AES). The fretting wear resistance of the film is tested by adopting a CETR UTM-2 type friction wear testing machine. The experimental conditions were: the motion mode is reciprocating type, room temperature air environment, and the mating part is a GCr15 steel ball with the diameter of 4.0 mm. The load range is 20-80N; the frequency range is 2-8 Hz; the temperature is 23-26 ℃. Friction environment: dry friction in the atmosphere or tank oil lubrication. And (3) testing a grinding mark profile curve of the surface of the sample by adopting a TR240 surface roughness meter, and calculating the wear volume of the film according to a wave trough on the curve.
Example 2:
the film prepared by Physical Vapor Deposition (PVD) mostly grows in a columnar crystal mode which is nearly vertical to the substrate, the crystal arrangement is dense, and the inter-crystal gap is narrow, so that the prepared film has high purity and compact structure. The prepared 2 kinds of films have compact tissues and uniform and flat surfaces. Through high power observation, the crystal grains are fine and reach the nanometer level. After the sulfurizing treatment, the crystal grains of the CrN/MoS2 composite film are further refined compared with the CrMoN composite film. Plays an important role in improving the hardness and the wear resistance of the film. Cr, Mo, N and S elements mainly exist on the surface of the CrN/MoS2 composite film, which shows that the S element can successfully permeate into the film through low-temperature ion sulfurization. Trace O elements can also be detected on the surface of the sample due to adsorption of atmospheric oxygen onto the surface of the composite membrane. Cr and Mo are in the average column transition group IV of the periodic table of elements, and the atomic radii are 0.1267 nm and 0.1454nm respectively. The N element having a small atomic radius and the transition metal form nitrides, and since the atomic radius ratio is less than 0.59, they can form only interstitial phases having a simple close-packed structure. The metal atoms are positioned on lattice nodes, and the N atoms are positioned in lattice gap positions due to smaller size. The sulfide generated by the S element and the metal has a hexagonal layered structure similar to graphite, so that the S element has excellent tribological properties.
Example 3:
when the sputtering rate is 50nm/min, the thickness of the sulfurizing layer of the CrN/MoS2 composite film reaches more than 500nm, the content of Cr, Mo and N elements gradually increases along with the increase of the depth and tends to be stable, and meanwhile, no Fe element exists in the composite film. The content of the S element is gradually reduced along with the increase of the depth; the O element is enriched on the surface of the film layer and is caused by slight oxidation of the surface layer of the film by air. In addition, the composition analysis of the film after 6min sputtering showed that: in the CrN/MoS2 composite film, the atomic fraction of Mo is about 22%, the atomic fraction of S is about 36%, and the atomic fractions of Cr and N are about 19% and 23%. The atomic ratio of Mo/S was about 0.6 and the atomic ratio of Cr/N was about 0.8, indicating that the film contained a small amount of MoN in addition to the stoichiometric ratio of MoS2 and CrN.
Example 4:
under the dry friction condition, the friction coefficients of the 2 films fluctuate sharply along with the change of the distance. The friction coefficient of the CrMoN composite membrane is higher than that of a CrN/MoS2 composite membrane, and the addition of the S element can generate a MoS2 lubricating phase, so that the friction coefficient of the CrMoN composite membrane can be effectively reduced. Compared with the dry friction condition, under the oil lubrication condition, the friction coefficients of the 2 films are obviously reduced, the fluctuation along with the change of the distance is relatively stable, and the friction coefficient of the CrN/MoS2 composite film is still smaller than that of the CrMoN composite film. Under the conditions of dry friction and oil lubrication, the abrasion volume values of the 2 films are all in the following order: CrMoN is more than CrN/MoS2, which shows that the CrN/MoS2 composite film has higher sliding wear resistance. Compared with the dry friction condition, under the oil lubrication condition, the friction coefficient and the wear volume of the 2 films are obviously reduced, wherein the wear volume value is reduced by 1 order of magnitude compared with that under the dry friction condition, and meanwhile, the friction coefficient difference value and the wear volume difference value of the 2 films are reduced, which shows that the friction coefficient is reduced, and the wear loss of the films can be effectively reduced. Further comparing and analyzing the wear volumes of the CrMoN composite membrane and the CrN/MoS2 composite membrane samples under the dry friction and oil lubrication conditions, so that the wear volume of the CrMoN composite membrane is about 3 times that of the CrN/MoS2 composite membrane under the dry friction condition; under the condition of oil lubrication, the wear volume of the CrMoN composite membrane is about 2 times of that of the CrN/MoS2 composite membrane. The wear of the CrMoN composite film is aggravated and the wear amount is increased under dry friction; and the CrN/MoS2 composite film has relatively good dry friction resistance.
Example 5:
during dry friction, the surface of a CrMoN film grinding mark is wide and deep in furrows, the signs of abrasive wear are obvious, meanwhile, more serious adhesive wear and fatigue wear shedding occur, even tearing occurs, the signs of plastic deformation to a certain extent are presented, and the wear weight loss is larger; the surface of a wear scar of the CrN/MoS2 composite film is relatively smooth, and the surface of the wear scar has a plurality of furrows which are left after the wear of abrasive grains and is flat, shallow and fine. Under the condition of oil lubrication, the wear marks of the 2 films are shallow and small in width, the wear surfaces are smooth and flat, very shallow and fine scratches are distributed on the surfaces, and the wear mechanisms of the two films are abrasive wear. Oil lubrication can significantly reduce surface wear of various films. Corresponding to the abrasion performance, in the 2 films, the abrasion surface of the CrN/MoS2 composite film with better abrasion performance has shallow furrow and smaller abrasion trace width; in the CrMoN composite membrane with weaker wear resistance, the wear mechanism is changed from the combined action of abrasive particle wear and adhesive wear under the dry friction condition to abrasive particle wear under the oil lubrication condition.

Claims (4)

1. A CrN/MoS2 solid self-lubricating composite membrane is prepared from the following raw materials: reagents used for synthesis of nano MoS 2: sodium molybdate (A.R) (Shanghai colloid chemical plant), hydroxylamine hydrochloride (A.R), thiourea (A.R) (Standard science and technology Co., Ltd., Tianjin), and absolute ethyl alcohol (A.R) (chemical reagent Co., Ltd., national drug group).
2. The CrN/MoS2 solid self-lubricating composite film according to claim 1, wherein the preparation steps of the CrN/MoS2 solid self-lubricating composite film are as follows: using a magnetron sputtering apparatus at N2Co-sputtering a Cr target and a Mo target in the atmosphere, depositing a CrMoN composite film on the surface of stainless steel, wherein the thickness of the CrMoN composite film is 5-6 mu m, and performing low-temperature (230 ℃) ion sulfurization treatment on the surface of the film for 2 hours by using sulfur vapor as a sulfurization source by using high-frequency pulse plasma diffusion equipment to prepare the CrN/MoS2 solid self-lubricating composite film.
3. The CrN/MoS2 solid self-lubricating composite film according to claim 1, wherein the CrN/MoS2 solid self-lubricating composite film is detected by the following steps: observing the surface morphology and the grinding trace morphology of the film by using a Philips Quant200 Scanning Electron Microscope (SEM), analyzing the microstructure and the frictional wear mechanism of the composite film, analyzing the chemical components of a sulfur-permeating layer by using a Genesis type energy spectrometer (EDS), analyzing the chemical components of the sulfur-permeating layer by using an ESCALB 250Xi type X-ray photoelectron spectrometer (XPS), and exciting a source: al target, fine sweep width: 25eV, analyzing the cross section component distribution of the CrN-based solid self-lubricating composite membrane by a PHI700 Auger Electron Spectrometer (AES), and testing the fretting wear resistance of the membrane by a CETR UTM-2 type friction wear testing machine under the following experimental conditions: the motion mode is reciprocating type, room temperature air environment, the mating part is GCr15 steel ball with diameter of 4.0mm, and the load range is 20-80N; the frequency range is 2-8 Hz; temperature 23-26 ℃, friction environment: and (3) dry friction in the atmosphere or lubrication of tank machine oil, testing a grinding trace profile curve of the surface of the sample by adopting a TR240 surface roughness meter, and calculating the wear volume of the film according to a wave trough on the curve.
4. The CrN/MoS2 solid self-lubricating composite film according to claim 1, wherein the CrMoN composite film is successfully prepared by magnetron sputtering technology, and low-temperature ion sulfurization treatment is carried out on the surface of the film by using high-frequency pulse plasma diffusion equipment, so that the CrN/MoS2 solid self-lubricating composite film containing MoS2 lubricating phase is successfully prepared, 2 films are compact and flat columnar crystal structures, and the grain size reaches the nanometer level; the CrN/MoS2 solid self-lubricating composite film is characterized in that a layered MoS2 soft phase is embedded in a (Cr, Mo) N hard phase to form a novel concrete structural film, the thickness of the CrN/MoS2 solid self-lubricating composite film is about 500nm, the CrN/MoS2 solid self-lubricating composite film mainly comprises Cr, Mo, N and S4 elements, a sulfurization product of the CrN/MoS2 solid self-lubricating composite film mainly comprises a MoS2 lubricating phase, the main phase structure of the CrN/MoS2 solid self-lubricating composite film comprises CrN, MoS2 and a small amount of MoN, and compared with the dry friction condition, the friction coefficients of 2 films are obviously reduced under the oil lubricating condition, the fluctuation along with the change of the distance is relatively stable, the abrasion volume is reduced by 1 order under the dry friction condition: CrMoN is more than CrN/MoS2, which shows that the CrN/MoS2 solid self-lubricating composite film has higher sliding wear resistance, abrasive wear of the CrN/MoS2 solid self-lubricating composite film occurs no matter under dry friction or oil lubrication conditions, the wear degree is lighter than that of the CrMoN composite film, the wear resistance and the friction reduction performance of the CrN/MoS2 solid self-lubricating composite film are greatly improved by the MoS2 lubricating phase synthesized in the composite film, and the CrMoN composite film even has serious adhesive wear under the dry friction condition; under the condition of oil lubrication, the surface wear of the 2 films is greatly reduced, so that the wear resistance and abrasion resistance of the films can be effectively improved under the condition of oil lubrication.
CN201811148943.3A 2018-09-29 2018-09-29 CrN/MoS2 solid self-lubricating composite film Pending CN110965015A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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CN113061858A (en) * 2021-03-15 2021-07-02 陕西科技大学 CrMoN/MoS2Wide-temperature-range lubricating wear-resistant composite film and preparation method thereof
CN113699483A (en) * 2021-08-31 2021-11-26 东风商用车有限公司 Surface treatment technology of gear and gear
CN114807833A (en) * 2022-04-20 2022-07-29 西安致远航空科技有限公司 Metal mold surface treatment process
CN114959578A (en) * 2022-06-22 2022-08-30 贵州西工液压有限公司 Surface treatment process for high-speed rail rim

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113061858A (en) * 2021-03-15 2021-07-02 陕西科技大学 CrMoN/MoS2Wide-temperature-range lubricating wear-resistant composite film and preparation method thereof
CN113699483A (en) * 2021-08-31 2021-11-26 东风商用车有限公司 Surface treatment technology of gear and gear
CN114807833A (en) * 2022-04-20 2022-07-29 西安致远航空科技有限公司 Metal mold surface treatment process
CN114807833B (en) * 2022-04-20 2023-08-25 西安致远航空科技有限公司 Metal mold surface treatment process
CN114959578A (en) * 2022-06-22 2022-08-30 贵州西工液压有限公司 Surface treatment process for high-speed rail rim

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