CN115466924B - Rolling contact fatigue resistant film on surface of gear bearing group and preparation method thereof - Google Patents
Rolling contact fatigue resistant film on surface of gear bearing group and preparation method thereof Download PDFInfo
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Classifications
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
- C23C14/022—Cleaning or etching treatments by means of bombardment with energetic particles or radiation
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/06—Alloys based on chromium
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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
- C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
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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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
- C23C14/325—Electric arc evaporation
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/70—Wind energy
- Y02E10/72—Wind turbines with rotation axis in wind direction
Abstract
The invention discloses a rolling contact fatigue resistant film on the surface of a gear bearing group and a preparation method thereof. The film provided by the invention has good binding force by adopting a mode of combining multi-arc ion plating and magnetron sputtering, and Ti element is introduced by changing the film preparation mode, so that on one hand, the wear resistance of the film is improved, on the other hand, the metal doped DLC film is obtained, and a good rolling contact fatigue performance effect is achieved.
Description
Technical Field
The invention relates to the technical field of surface engineering, relates to a surface wear-resistant rolling contact fatigue protection method for torque transmission components such as an aeroengine gear bearing group and the like, and in particular relates to a rolling contact fatigue resistant film for the surface of a gear bearing group and a preparation method thereof.
Background
The gear is used as an important rotating part in mechanical equipment, can transfer the rotation of one shaft to the other shaft, can realize actions such as speed reduction, speed increase, direction change, reversing and the like, and is also one of important fault sources. In recent years, the primary failure modes of gears have been associated with micropitting, wear, yellowing, abrasion, smearing, and macroscopic pitting, all of which occur at or near the surface. Thus, to prevent these tribological failures, various surface engineering methods are currently being considered to deposit wear resistant films to alter the surface characteristics of such bearings and gears.
However, the wear-resistant film on the surface of the gear is in the complex working conditions of high load, high speed, high temperature and the like for a long time, and the film is subjected to complex alternating stress and shearing stress for a long time. Therefore, the film is extremely easy to distort, generate defects, initiate cracks and microcrack expansion under the comprehensive action of the conditions until the film is peeled off to cause surface damage (contact fatigue failure) under the condition of contact, and the structure of the gear set in operation is seriously influenced and even the gear set is damaged. It is therefore critical for the relevant investigation of rolling contact fatigue failure of the surface wear-resistant or lubricating coating of gears, bearing sets.
A diamond-like film, english Diamond like Carbon, DLC for short, which is an amorphous carbon film with properties very similar to diamond. Has properties similar to those of diamond, such as high hardness, low friction coefficient, high elastic modulus, high resistivity, good acoustic properties, high infrared transmittance, etc., and is therefore a very promising material. Along with the change of the preparation method and a series of doping elements, the properties and the structures of the prepared DLC film are greatly different, and meanwhile, the phenomenon of film falling can be caused due to the fact that the internal stress and the thermal stress existing in the DLC body are large. Therefore, reducing internal stress and thermal stress existing in the DLC film is one of the key problems to be solved by the DLC film while ensuring good rolling contact fatigue resistance and wear resistance of the film.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a rolling contact fatigue resistant film on the surface of a gear bearing group and a preparation method thereof.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a rolling contact fatigue resistant film on the surface of a gear bearing group comprises a metal Cr bottom layer, a CrTi metal transition layer, a Ti-C nano transition layer and a Ti-DLC functional layer which are arranged from bottom to top.
Further, the metal Cr bottom layer comprises Cr;
the CrTi metal transition layer comprises Cr and Ti, wherein the atomic percentage at% of Cr:72.5%, ti:27.5%;
the Ti-C nano transition layer comprises C and Ti, wherein the C is as follows in atom percent: 81.3%, ti:18.7%;
the Ti-DLC functional layer comprises C and Ti, wherein the C is as follows in atom percent: 55.1 to 98.5 percent of Ti:1.5 to 44.9 percent.
Further, the thickness of the metal Cr bottom layer is 0.3-0.5 mu m;
the thickness of the CrTi metal transition layer is 0.1-0.15 mu m;
the thickness of the Ti-C nano transition layer is 0.05-0.1 mu m;
the thickness of the Ti-DLC functional layer is 1.3-2.0 mu m.
The preparation method of the rolling contact fatigue resistant film on the surface of the gear bearing group comprises the following steps:
s1, carrying out ion etching on the surface of a substrate by adopting a radio frequency ion source in an argon atmosphere, then depositing Cr, and forming a metal Cr bottom layer on the surface of the substrate;
s2, synchronously performing first direct-current magnetron sputtering and multi-arc ion plating deposition on the surface of the metal Cr bottom layer in an argon atmosphere to obtain a CrTi metal transition layer;
s3, synchronously performing first direct current magnetron sputtering and second direct current magnetron sputtering on the surface of the CrTi metal transition layer in an argon atmosphere to obtain a Ti-C nano transition layer;
s4, synchronously performing first direct current magnetron sputtering and second direct current magnetron sputtering on the surface of the Ti-C nano transition layer in an argon atmosphere to obtain a Ti-DLC functional layer, and forming the rolling contact fatigue resistant film on the surface of the gear bearing group.
Further, in the step S1, the process parameters for depositing Cr include: the bias voltage is 100-400V, the pure Cr target arc current is 100A, and the time is 25-40 min.
Further, in the ion etching in the step S1, the ion source voltage is set to be 500V, the duty ratio is 50%, the vacuum degree is 0.3-0.7 Pa, the bias voltage is 600-800V, and the etching time is 20-30 min.
Further, in the step S2, the process parameters of synchronously performing the first dc magnetron sputtering and the multi-arc ion plating deposition on the surface of the metal Cr bottom layer include: the bias voltage is 100V, the Cr target arc current is 100A, the first direct current magnetron sputtering target current is 2.5A, and the time is 10-25 min.
Further, in the step S3, the process parameters of the first dc magnetron sputtering and the second dc magnetron sputtering include: bias voltage is 100V, the first DC magnetron sputtering target current is 2.5A, the second DC magnetron sputtering target current is 3.0A, and time is 20min.
Further, in the step S4, the technological parameters of performing the first dc magnetron sputtering and the second dc magnetron sputtering on the surface of the Ti-C nano transition layer simultaneously include: bias voltage is 100V, the first DC magnetron sputtering target current is 2.5A, the second DC magnetron sputtering target current is 3.0-7.0A, and the time is 60-150 min.
Further, in step S2, the target material deposited by multi-arc ion plating is a metal Cr target; the target material of the first direct current magnetron sputtering in the step S2 and the step S3 is a Ti target; and in the step S3, the target material of the second direct current magnetron sputtering is a graphite target.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a rolling contact fatigue resistant film on the surface of a gear bearing group, which has good binding force. By introducing Ti element, on one hand, the doped metal atoms form clusters in the DLC film matrix, so that the toughness of the DLC film can be remarkably improved, and meanwhile, the internal stress is released through plastic deformation. On the other hand, when a trace amount of Ti is doped, the existence of TiC nano microcrystals can adjust the film structure, improve the hardness and fracture toughness of the DLC film, ensure that the DLC film has excellent tribology performance, and obviously improve the performance of the film in rolling contact.
The invention combines industrial multi-arc ion plating and magnetron sputtering technology, and utilizes vacuum vapor deposition technology to deposit Ti-DLC composite film on the surface of stainless steel matrix. Compared with a single vapor deposition technology, the composite vapor deposition technology is used for depositing the films on the same batch of samples, so that the cleanliness degree of the films in the deposition process can be ensured, and the prepared films are more excellent in performance. The film provided by the invention has good binding force, ti element is introduced by changing the film preparation mode, so that on one hand, the wear resistance of the film is improved, and on the other hand, the metal doped DLC film is obtained, and a good rolling contact fatigue performance effect is achieved.
Furthermore, before the film is deposited, the substrate is pretreated by adopting an ion etching technology and an anti-sputtering technology, so that impurities and pollutants adsorbed on the surface of the substrate can be cleaned more effectively, a relatively rough surface structure is generated on the surface of the substrate, and the binding force between the film and the substrate is enhanced.
Furthermore, the rolling contact fatigue resistant film prepared on the surface of the stainless steel and taking the Ti-DLC functional layer as the outer layer realizes the more stable rolling contact fatigue resistant protection effect on the gear bearing group in the daily service and maintenance process of the gear bearing group of the engine through the control of metal and nonmetal targets and deposition conditions.
Drawings
FIG. 1 is a schematic diagram of a multi-arc ion plating composite DC magnetron sputtering apparatus employed in the present invention;
FIG. 2 is a schematic diagram of a chamber of a multi-arc ion plating composite DC magnetron sputtering apparatus employed in the present invention;
FIG. 3 is a schematic structural view of the rolling contact fatigue resistant film provided by the invention;
FIG. 4 is a scanning electron microscope photograph of the surface morphology and element distribution map of the rolling contact fatigue resistant film prepared on the surface of the stainless steel substrate provided in example 1; wherein, (a) is the surface morphology, (b) is Ti element, (C) is C element, and (d) is Cr element;
FIG. 5 shows the surface Scanning Electron Microscope (SEM) spectrum element content of the rolling contact fatigue resistant film prepared on the surface of the stainless steel substrate according to example 1;
FIG. 6 is a graph showing the nano-indentation load displacement curve as a test result of the nano-mechanical measurement system of the rolling contact fatigue resistant film provided in example 2;
FIG. 7 is a diffraction pattern of a Raman spectrometer of a rolling contact fatigue resistant film prepared on the surface of a stainless steel substrate provided in example 2;
FIG. 8 is a press-in test result of the film-based interfacial bonding property of the rolling contact fatigue resistant film prepared on the surface of the stainless steel substrate provided in example 2;
FIG. 9 is a graph showing the comparison of rolling contact fatigue life in a test of a rolling contact fatigue resistant film prepared according to the present invention:
FIG. 10 shows the stress distribution test results of the rolling contact fatigue resistant film prepared by the present invention.
In the figure, 1 is a metal Cr bottom layer, 2 is a CrTi metal transition layer, 3 is a Ti-C nano transition layer, 4 is a Ti-DLC functional layer, 5 is a chamber, 6 is a rotating frame, 7 is a maintenance pump, 8 is a molecular pump, 9 is a high valve, 10 is a grating, 11 is a front valve, 12 is a Roots pump, 13 is a mechanical pump, 14 is a rough pumping valve, and 15 is a bleed valve.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and examples, but the examples are not to be construed as limiting the scope of the present invention.
It should be noted that, the experimental methods described in the following examples are all conventional methods unless otherwise specified; the reagents and materials employed, unless otherwise specified, are commercially available.
The purity of the target metal Cr target adopted by each embodiment of the invention is 99.99 percent, the purity of the magnetic control graphite target is 99.999 percent, and the purity of the magnetic control target Ti is 99.99 percent.
The following embodiment of the invention is a multi-arc ion plating composite direct current magnetron sputtering device used in the preparation of a rolling contact fatigue resistant film, and is shown in fig. 1 and 2, and the device comprises a chamber 5, a maintenance pump 7, a molecular pump 8, a high valve 9, a grating 10, a front valve 11, a Roots pump 12, a mechanical pump 13, a rough pumping valve 14 and a deflation valve 15; wherein, a deflation valve 15 is arranged on the chamber 5, one end of the molecular pump 8 connects the high valve 9 with the chamber 5, and a grating 10 is arranged on a pipeline between the high valve 9 and the chamber 5; the other end of the molecular pump 8 and the maintaining pump 7 are connected with one end of the front valve 11, the other end of the front valve 11 is divided into two paths, one path is connected with the cavity 5 through the rough pumping valve 14, and the other path is connected with the mechanical pump 13 through the Roots pump 12.
The pump 7 is used for maintaining the forevacuum of the molecular pump 8, the Roots pump 12, the mechanical pump and the rough pumping valve 14 form a low vacuum acquisition path, and the mechanical pump 13 and the Roots pump 12 are connected with the molecular pump 8 and the high valve 9 through the pre-valve 11 to form a high vacuum acquisition path. The equipment comprises a rotating frame 6 arranged in a cavity 5, wherein four multi-arc ion arc plating targets (a first arc target, a second arc target, a third arc target and a fourth arc target), two direct current magnetic control targets (a first magnetic control target and a second magnetic control target), an armored heating rod and a radio frequency ion source are simultaneously arranged in the cavity 5, and exciting coils are respectively arranged behind the 4 multi-arc ion arc plating targets; the invention takes the first arc target and the second arc target as a multi-arc ion plating target source; the first magnetron target (Ti metal target) is used as a first direct current magnetron sputtering target source, and the second magnetron target (graphite target) is used as a second direct current magnetron sputtering target source.
Preferably, the rotating frame 2 rotates around the center, and meanwhile, the rotating frame 2 is additionally arranged, so that planetary rotation is realized on the experimental sample. By adopting the mode, the influence caused by the placement of the target can be obviously eliminated, so that the thickness of the deposited film and the element distribution are more uniform.
The invention provides a rolling contact fatigue resistant film on the surface of a gear bearing group, which is shown in figure 3, and comprises a metal Cr bottom layer 1, a CrTi metal transition layer 2, a Ti-C nano transition layer 3 and a Ti-DLC functional layer 4 which are arranged on the surface of a stainless steel surface matrix from bottom to top;
the metal Cr bottom layer 1 comprises Cr;
the CrTi metal transition layer 2 comprises Cr and Ti, wherein the atomic percentage at% of Cr:72.5%, ti:27.5%;
the Ti-C nano transition layer 3 comprises C and Ti, wherein at% is C:81.3%, ti:18.7%;
the Ti-DLC functional layer 4 comprises C and Ti, wherein at% is C:55.1 to 98.5 percent of Ti:1.5 to 44.9 percent.
The thickness of the metal Cr bottom layer 1 is 0.3-0.5 mu m, the thickness of the CrTi metal transition layer 2 is 0.1-0.15 mu m, the thickness of the Ti-C nano transition layer 3 is 0.05-0.1 mu m, and the thickness of the Ti-DLC functional layer 4 is 1.3-2.0 mu m.
The substrate selected in each of the examples below was 304 stainless steel.
The preparation method of the rolling contact fatigue resistant film on the surface of the gear bearing group comprises the following steps:
s1, performing pretreatment such as acetone and alcohol cleaning on the surface of a stainless steel substrate;
s2, in an argon atmosphere, carrying out ion etching on the surface of the substrate by adopting a radio frequency ion source, and then depositing a metal Cr bottom layer 1 on the surface of the substrate by adopting multi-arc ion plating deposition;
in the step S2, the preparation process parameters of the metal Cr underlayer 1 include: the time is 25-40 min, the bias voltage is 100-400V, and the pure Cr target arc current is 100A.
More preferably, in the ion etching process in S2, the ion source voltage is set to be 500V, the duty ratio is 50%, the vacuum degree is 0.3-0.7 Pa, the bias voltage is 600-800V, and the etching time is 20-30 min.
S3, synchronously performing first direct-current magnetron sputtering and multi-arc ion plating deposition on the surface of the metal layer in the argon atmosphere at the vacuum degree of 0.5-0.6 Pa to obtain a CrTi metal transition layer 2;
in the step S3, the preparation process parameters of the CrTi metal transition layer 2 include: the time is 10-25 min, the bias voltage is 100V, the pure Cr target arc current is 100A, and the first direct current magnetron sputtering target current is 2.5A.
S4, synchronously performing first direct current magnetron sputtering and second direct current magnetron sputtering on the surface of the CrTi metal transition layer 2 in an argon atmosphere to obtain a Ti-C nano transition layer 3;
in the step S4, the preparation process parameters of the Ti-C nano transition layer 3 include: and the time is 20min, the bias voltage is 100V, the first direct current magnetron sputtering target current is 2.5A, and the second direct current magnetron sputtering target current is 3.0A.
S5, synchronously performing first direct current magnetron sputtering and second direct current magnetron sputtering on the surface of the Ti-C nano transition layer 3 in an argon atmosphere to obtain a Ti-DLC functional layer 4, and thus obtaining the rolling contact fatigue resistant film on the surface of the gear bearing group.
In the step S5, the preparation process parameters of the Ti-C nano transition layer 3 include: the time is 60-150 min, the bias voltage is 100V, the first direct current magnetron sputtering target current is 2.5A, and the second direct current magnetron sputtering target current is 3.0-7.0A. The target material deposited by the multi-arc ion plating is a metal Cr target; the target material of the first direct current magnetron sputtering is a Ti target; and the target material of the second direct current magnetron sputtering is a graphite target.
In the steps S3, S4 and S5, the flow rate of the argon gas is 125sccm.
The application of the composite film in the rolling contact fatigue and abrasion resistance of the surface of the gear bearing group.
Example 1
The rolling contact fatigue resistant film on the surface of the gear bearing group is shown in figure 3, and comprises a metal Cr bottom layer 1, a CrTi metal transition layer 2, a Ti-C nano transition layer 3 and a Ti-DLC functional layer 4 which are arranged on the surface of a stainless steel surface matrix from bottom to top;
the rolling contact fatigue resistant film on the surface of the gear bearing group is prepared according to the following steps:
(1) Will be of the size ofPolishing and cleaning pretreatment are respectively carried out on the round 304 stainless steel substrate;
the polishing is specifically as follows: and (3) removing the surface protection layer from the finished product 304 stainless steel substrate, and then finely polishing by adopting polishing cloth.
The cleaning is specifically as follows: and sequentially ultrasonically cleaning the polished substrate by adopting acetone and absolute ethyl alcohol, and then drying by using high-purity argon.
Placing the pretreated stainless steel substrate in a vacuum chamber of a multi-arc ion plating composite direct current magnetron sputtering device, and then fixing the stainless steel substrate on a planetary rotating frame;
(2) For the multi-arc ion plating composite direct current magnetron sputtering equipment, referring to fig. 1 and 2, the equipment comprises a low vacuum acquisition path consisting of a pump maintaining the forevacuum of a molecular pump, a Roots pump, a mechanical pump and a rough pumping valve, and a high vacuum acquisition path consisting of the mechanical pump and the Roots pump connected with the molecular pump through a forevalve and a high valve. In the process of vacuum acquisition, after the vacuum degree reaches a certain degree, a heat module (heating device) is opened to heat the cavity, and after the vacuum degree and the temperature reach certain requirements, a substrate is etched through an Ion module (radio frequency Ion source), in fig. 1, DC1 and DC2 are respectively a first magnetron sputtering and a second magnetron sputtering, and ARC1, ARC2, ARC3 and ARC4 respectively correspond to four ARC target sources of multi-ARC Ion plating. The subsequent process of film preparation is mainly carried out in a vacuum chamber which ensures vacuum degree and temperature.
Vacuumizing the vacuum chamber by adopting a mechanical pump and molecular pump mode until the vacuum degree is less than 2.5X10 -3 Pa, a heating device is opened to heat the vacuum cavity in the process of vacuum acquisition, and the heating temperature is set to be 200 ℃;
(3) Firstly, a radio frequency ion source is adopted to etch a substrate, and the specific process parameters are as follows: when the vacuum degree reaches < 2.5X10 -3 After Pa, rotating the rotating frame at a rotation speed of 15Hz, simultaneously introducing Ar gas into the vacuum cavity, setting the ion source voltage to be 500V, setting the duty ratio to be 50%, setting the Ar gas flow to be 140sccm, setting the grating angle to be 73 degrees, setting the vacuum degree to be 0.6Pa, and etching for 20-30 min; and then the ion source is closed, the first direct current magnetron sputtering is started, the current of the first direct current magnetron sputtering target is set to be 2.5A, the voltage is 300V, the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55-0.65 Pa, the bias voltage is 700V, and the reverse sputtering time is 5min. Then turning off the first direct current magnetron sputtering;
(4) After ion etching and anti-sputtering are finished, firstly, depositing metal Cr on the etched stainless steel substrate for 40min by adopting multi-arc ion plating to form a metal Cr bottom layer 1, wherein the thickness of the metal Cr bottom layer is 0.35 mu m. The Cr target current is 100A, the deposition time is 25min, the bias voltage is 100-400V, and the air pressure is 0.6Pa;
(5) And continuously depositing a CrTi metal transition layer 2 on the metal Cr bottom layer 1, regulating Ar gas flow to 125sccm, regulating a grating angle to 75 degrees, opening a first direct current magnetron sputtering target baffle plate, setting the target current of the first direct current magnetron sputtering target to 2.5A, setting the voltage to 300V, setting the Cr target current of the multi-arc ion arc plating target to 100A, and generating glow discharge on the first direct current magnetron sputtering target, wherein the direct current magnetron sputtering process is started. The multi-arc ion plating arc target source starts arc discharge, the multi-arc ion plating preparation process starts, the substrate bias voltage is set to be 100V, the deposition time is 10min, the deposition thickness is 0.1-0.15 um, and a CrTi metal transition layer 2 is formed;
(6) After depositing the CrTi metal transition layer 2, closing a first multi-arc ion arc plating target and a second multi-arc ion arc plating target, opening a second direct current magnetron sputtering target baffle, continuing to deposit the Ti-C nano transition layer 3, enabling Ar gas flow to be 125sccm, enabling a grating angle to be 75 degrees, enabling vacuum degree to be 0.55Pa, simultaneously starting the first direct current magnetron sputtering and the second direct current magnetron sputtering, setting Ti target current to be 2.5A, enabling voltage to be 300V, enabling graphite target current to be 3.0A, enabling voltage to be 525V, enabling substrate bias to be 100V, enabling deposition time to be 10min, enabling deposition thickness to be 0.05-0.1 um, and forming the Ti-C nano transition layer 3;
(7) And after the Ti-C nano transition layer 3 is deposited, continuously depositing a Ti-DLC functional layer 4, wherein the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55Pa, simultaneously, the first direct current magnetron sputtering and the second direct current magnetron sputtering are kept, the Ti target current is 2.5A, the voltage is 300V, the graphite target current is 4.0A, the voltage is 525V, the substrate bias is 100V, the deposition time is 150min, and the deposition thickness is 2.3um, so that the rolling contact fatigue resistant film on the surface of the gear bearing group is obtained.
Example 2
The rolling contact fatigue resistant film on the surface of the gear bearing group is shown in FIG. 3, and comprises a metal Cr bottom layer 1, a CrTi metal transition layer 2, a Ti-C nano transition layer 3 and a Ti-DLC functional layer 4 which are arranged on the surface of a stainless steel surface substrate from bottom to top;
the rolling contact fatigue resistant film on the surface of the gear bearing group is prepared according to the following steps:
(1) Will be of the size ofPolishing and cleaning the round 304 stainless steel substrate respectively; and sequentially ultrasonically cleaning the polished substrate by adopting acetone and absolute ethyl alcohol, and then drying by using high-purity argon.
Placing the pretreated stainless steel substrate in a vacuum chamber of a multi-arc ion plating composite direct current magnetron sputtering device, and then fixing the stainless steel substrate on a planetary rotating frame;
(2) Firstly, vacuumizing a vacuum chamber by adopting a mechanical pump and molecular pump mode until the vacuum degree is less than 2.5x10 -3 Pa, overreach in vacuumIn the process, a heating device is opened to heat the vacuum cavity, and the temperature is set to be 200 ℃;
(3) Firstly, etching a substrate by adopting a radio frequency ion source, setting the ion source voltage to be 500V, the duty ratio to be 50%, the Ar gas flow to be 140sccm, the grating angle to be 73 degrees, the vacuum degree to be 0.6Pa, and etching for 20-30 min; and then the ion source is closed, the first direct current magnetron sputtering is started, the current of the first direct current magnetron sputtering target is set to be 2.5A, the voltage is 300V, the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55-0.65 Pa, the bias voltage is 700V, and the reverse sputtering time is 5min. Then turning off the first direct current magnetron sputtering;
(4) After ion etching and anti-sputtering are finished, firstly, depositing metal Cr on the etched stainless steel substrate for 40min by adopting multi-arc ion plating to form a metal Cr bottom layer 1, wherein the thickness of the metal Cr bottom layer is 0.3-0.5 mu m. The Cr target current is 100A, the deposition time is 25min, the bias voltage is 100-400V, and the air pressure is 0.6Pa;
(5) Depositing a CrTi metal transition layer 2 on a metal Cr bottom layer 1, regulating Ar gas flow to 125sccm, regulating grating angle to 75 degrees, regulating vacuum degree to 0.55Pa, opening a first direct current magnetron sputtering target baffle, setting target current to 2.5A, setting voltage to 300V, setting Cr target current to 100A, setting substrate bias to 100V, setting deposition time to 10min, and setting deposition thickness to 0.1-0.15 um;
(6) Continuously depositing a Ti-C nano transition layer 3 on the CrTi metal transition layer 2, wherein the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55Pa, simultaneously starting a first direct current magnetron sputtering and a second direct current magnetron sputtering, setting the Ti target current to 2.5A, the voltage to 300V, the graphite target current to 3.0A, the voltage to 525V, the substrate bias voltage to 100V, the deposition time to 10min, and the deposition thickness to 0.05-0.1 um;
(7) And continuously depositing a Ti-DLC functional layer 4 on the deposited Ti-C nano transition layer 3, wherein the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55Pa, meanwhile, the first direct current magnetron sputtering and the second direct current magnetron sputtering are kept, the Ti target current is 2.5A, the voltage is 300V, the graphite target current is 3.6A, the voltage is 525V, the substrate bias is 100V, the deposition time is 180 minutes, and the deposition thickness is 2.2um, so that the rolling contact fatigue resistant film on the surface of the gear bearing group is obtained.
Example 3
The same as in example 1, except that in step (7) in this example, the deposition time was 180min.
Example 4
The same as in example 2, except that in step (7) in this example, the Ti target current was set to 2.2A.
Example 5
(1) Firstly, a radio frequency ion source is adopted to etch a substrate, and the specific process parameters are as follows: when the vacuum degree reaches < 2.5X10 -3 After Pa, rotating the rotating frame at a rotation speed of 15Hz, simultaneously introducing Ar gas into the vacuum cavity, setting the ion source voltage to be 500V, setting the duty ratio to be 50%, setting the Ar gas flow to be 140sccm, setting the grating angle to be 73 degrees, setting the vacuum degree to be 0.3Pa, and etching for 30min; and then the ion source is closed, the first direct current magnetron sputtering is started, the current of the first direct current magnetron sputtering target is set to be 2.5A, the voltage is 300V, the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55Pa, the bias voltage is 600V, and the reverse sputtering time is 5min. Then turning off the first direct current magnetron sputtering;
after ion etching and anti-sputtering are finished, firstly, depositing metal Cr on the etched stainless steel substrate for 40min by adopting multi-arc ion plating to form a metal Cr bottom layer 1, wherein the thickness of the metal Cr bottom layer is 0.35 mu m. The Cr target current is 100A, the deposition time is 25min, the bias voltage is 100V, and the air pressure is 0.6Pa;
(2) And continuously depositing a CrTi metal transition layer 2 on the metal Cr bottom layer 1, regulating Ar gas flow to 125sccm, regulating a grating angle to 75 degrees, opening a first direct current magnetron sputtering target baffle plate, setting the target current of the first direct current magnetron sputtering target to 2.5A, setting the voltage to 300V, setting the Cr target current of the multi-arc ion arc plating target to 100A, and generating glow discharge on the first direct current magnetron sputtering target, wherein the direct current magnetron sputtering process is started. The multi-arc ion plating arc target source starts arc discharge, the multi-arc ion plating preparation process starts, the substrate bias voltage is set to be 100V, the deposition time is 10min, the deposition thickness is 0.1-0.15 um, and a CrTi metal transition layer 2 is formed;
(3) After depositing the CrTi metal transition layer 2, closing a first multi-arc ion arc plating target and a second multi-arc ion arc plating target, opening a second direct current magnetron sputtering target baffle, continuing to deposit the Ti-C nano transition layer 3, enabling Ar gas flow to be 125sccm, enabling a grating angle to be 75 degrees, enabling vacuum degree to be 0.55Pa, simultaneously starting the first direct current magnetron sputtering and the second direct current magnetron sputtering, setting Ti target current to be 2.5A, enabling voltage to be 300V, enabling graphite target current to be 3.0A, enabling voltage to be 525V, enabling substrate bias to be 100V, enabling deposition time to be 10min, enabling deposition thickness to be 0.05-0.1 um, and forming the Ti-C nano transition layer 3;
(4) And after the Ti-C nano transition layer 3 is deposited, continuously depositing a Ti-DLC functional layer 4, wherein the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55Pa, simultaneously, the first direct current magnetron sputtering and the second direct current magnetron sputtering are kept, the Ti target current is 2.5A, the voltage is 300V, the graphite target current is 3.0A, the voltage is 525V, the substrate bias is 100V, the deposition time is 60min, and the deposition thickness is 2.3um, so that the rolling contact fatigue resistant film on the surface of the gear bearing group is obtained.
Example 6
(1) Firstly, a radio frequency ion source is adopted to etch a substrate, and the specific process parameters are as follows: when the vacuum degree reaches < 2.5X10 -3 After Pa, rotating the rotating frame at a rotation speed of 15Hz, simultaneously introducing Ar gas into the vacuum cavity, setting the ion source voltage to be 500V, setting the duty ratio to be 50%, setting the Ar gas flow to be 140sccm, setting the grating angle to be 73 degrees, setting the vacuum degree to be 0.7Pa, and etching for 25min; and then the ion source is closed, the first direct current magnetron sputtering is started, the current of the first direct current magnetron sputtering target is set to be 2.5A, the voltage is 300V, the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.65Pa, the bias voltage is 700V, and the reverse sputtering time is 5min. Then turning off the first direct current magnetron sputtering;
after ion etching and anti-sputtering are finished, firstly, depositing metal Cr on the etched stainless steel substrate for 40min by adopting multi-arc ion plating to form a metal Cr bottom layer 1, wherein the thickness of the metal Cr bottom layer is 0.3-0.5 mu m. The Cr target current is 100A, the deposition time is 40min, the bias voltage is 400V, and the air pressure is 0.6Pa;
(2) And continuously depositing a CrTi metal transition layer 2 on the metal Cr bottom layer 1, regulating Ar gas flow to 125sccm, regulating a grating angle to 75 degrees, opening a first direct current magnetron sputtering target baffle plate, setting the target current of the first direct current magnetron sputtering target to 2.5A, setting the voltage to 300V, setting the Cr target current of the multi-arc ion arc plating target to 100A, and generating glow discharge on the first direct current magnetron sputtering target, wherein the direct current magnetron sputtering process is started. The multi-arc ion plating arc target source starts arc discharge, the multi-arc ion plating preparation process starts, the substrate bias voltage is set to be 100V, the deposition time is 10min, the deposition thickness is 0.1-0.15 um, and a CrTi metal transition layer 2 is formed;
(3) After depositing the CrTi metal transition layer 2, closing a first multi-arc ion arc plating target and a second multi-arc ion arc plating target, opening a second direct current magnetron sputtering target baffle, continuing to deposit the Ti-C nano transition layer 3, enabling Ar gas flow to be 125sccm, enabling a grating angle to be 75 degrees, enabling vacuum degree to be 0.55Pa, simultaneously starting the first direct current magnetron sputtering and the second direct current magnetron sputtering, setting Ti target current to be 2.5A, enabling voltage to be 300V, enabling graphite target current to be 3.0A, enabling voltage to be 525V, enabling substrate bias to be 100V, enabling deposition time to be 10min, enabling deposition thickness to be 0.05-0.1 um, and forming the Ti-C nano transition layer 3;
(4) And after the Ti-C nano transition layer 3 is deposited, continuously depositing a Ti-DLC functional layer 4, wherein the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55Pa, meanwhile, the first direct current magnetron sputtering and the second direct current magnetron sputtering are kept, the Ti target current is 2.5A, the voltage is 300V, the graphite target current is 7.0A, the voltage is 525V, the substrate bias is 100V, the deposition time is 100min, and the deposition thickness is 2.3um, so that the rolling contact fatigue resistant film on the surface of the gear bearing group is obtained.
Example 7
(1) Firstly, a radio frequency ion source is adopted to etch a substrate, and the specific process parameters are as follows: when the vacuum degree reaches < 2.5X10 -3 After Pa, rotating the rotating frame at a rotation speed of 15Hz, simultaneously introducing Ar gas into the vacuum cavity, setting the ion source voltage to be 500V, setting the duty ratio to be 50%, setting the Ar gas flow to be 140sccm, setting the grating angle to be 73 degrees, setting the vacuum degree to be 0.5Pa, and etching for 25min; and then the ion source is closed, the first direct current magnetron sputtering is started, the current of the first direct current magnetron sputtering target is set to be 2.5A, the voltage is 300V, the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.6Pa, the bias voltage is 700V, and the reverse sputtering time is 5min. Then turning off the first direct current magnetron sputtering;
after ion etching and anti-sputtering are finished, firstly, depositing metal Cr on the etched stainless steel substrate for 40min by adopting multi-arc ion plating to form a metal Cr bottom layer 1, wherein the thickness of the metal Cr bottom layer is 0.3-0.5 mu m. The Cr target current is 100A, the deposition time is 35min, the bias voltage is 200V, and the air pressure is 0.6Pa;
(2) And continuously depositing a CrTi metal transition layer 2 on the metal Cr bottom layer 1, regulating Ar gas flow to 125sccm, regulating a grating angle to 75 degrees, opening a first direct current magnetron sputtering target baffle plate, setting the target current of the first direct current magnetron sputtering target to 2.5A, setting the voltage to 300V, setting the Cr target current of the multi-arc ion arc plating target to 100A, and generating glow discharge on the first direct current magnetron sputtering target, wherein the direct current magnetron sputtering process is started. The multi-arc ion plating arc target source starts arc discharge, the multi-arc ion plating preparation process starts, the substrate bias voltage is set to be 100V, the deposition time is 10min, the deposition thickness is 0.1-0.15 um, and a CrTi metal transition layer 2 is formed;
(3) After depositing the CrTi metal transition layer 2, closing a first multi-arc ion arc plating target and a second multi-arc ion arc plating target, opening a second direct current magnetron sputtering target baffle, continuing to deposit the Ti-C nano transition layer 3, enabling Ar gas flow to be 125sccm, enabling a grating angle to be 75 degrees, enabling vacuum degree to be 0.55Pa, simultaneously starting the first direct current magnetron sputtering and the second direct current magnetron sputtering, setting Ti target current to be 2.5A, enabling voltage to be 300V, enabling graphite target current to be 3.0A, enabling voltage to be 525V, enabling substrate bias to be 100V, enabling deposition time to be 10min, enabling deposition thickness to be 0.05-0.1 um, and forming the Ti-C nano transition layer 3;
(4) And after the Ti-C nano transition layer 3 is deposited, continuously depositing a Ti-DLC functional layer 4, wherein the Ar gas flow is 125sccm, the grating angle is 75 degrees, the vacuum degree is 0.55Pa, simultaneously, the first direct current magnetron sputtering and the second direct current magnetron sputtering are kept, the Ti target current is 2.5A, the voltage is 300V, the graphite target current is 5.0A, the voltage is 525V, the substrate bias is 100V, the deposition time is 120min, and the deposition thickness is 2.3um, so that the rolling contact fatigue resistant film on the surface of the gear bearing group is obtained.
In order to illustrate the relative performance of the rolling contact fatigue resistant film and the preparation method provided by the invention, the relative characterization test is carried out on the embodiment 1 to 3, and the method is shown in fig. 4 to 8.
Fig. 4 is a scanning electron micrograph of the surface morphology of the rolling contact fatigue resistant film prepared on the stainless steel surface provided in example 1 and an element content graph, and as can be seen from fig. 4 (a), (b), (c) and (d), C, ti elements in the film are uniformly distributed, which indicates that Ti element is well distributed in the DLC film during the co-deposition process.
Fig. 5 is a graph showing the element content of the surface topography scan of the rolling contact fatigue resistant film prepared on the stainless steel surface provided in example 1, and as can be seen from fig. 5, the element content of C, ti in the film is 78.3% and 14.2%, respectively.
Fig. 6 is a graph of the results of a surface raman spectrum test of a rolling contact fatigue resistant film prepared on the surface of a stainless steel provided in example 2, wherein in fig. 6, D, G and a11 correspond to different peaks of the raman spectrum of the film, the relative intensity of the D band is a reflection of the degree of disorder of the crystal structure, the G band represents a first-order scattering E2G vibration mode, which is used for characterizing the Sp2 bond structure of carbon, a11 represents the total spectrum of the raman spectrum of the film, and the D/G intensity ratio is a measurement means of disordered graphite. As can be seen from FIG. 6, the phase composition in the film is mainly Sp of C 2 The phase is mainly, the graphite phase in the film exists more, and the self-lubricating performance of the film is good. And the nanometer indentation load displacement curve of the film can be seen, so that the hardness and the elastic modulus change of the film can be analyzed and tested.
FIG. 7 is a graph of the nano-indentation load displacement of a film, which can be analyzed to determine the change in hardness and elastic modulus of the film. As can be seen from fig. 7, the film hardness is relatively low, the elastic modulus is high, and the film characteristics such as a tough film are exhibited.
Fig. 8 is a graph of the press-in test result of the rolling contact fatigue resistant film prepared on the stainless steel surface provided in example 2, and as can be seen from fig. 8, the film and the stainless steel substrate have good performance, and can be well applied to practical working conditions.
Fig. 9 is a graph showing the rolling contact test results of rolling contact fatigue resistant films prepared on the stainless steel surfaces provided in examples 1, 2 and 3, and it is known from fig. 9 that the rolling contact fatigue resistant films can well resist rolling contact fatigue and further protect the gear and the bearing substrate in practical working conditions.
Fig. 10 is a graph showing the stress test results of the rolling contact resistant film prepared on the stainless steel surface in example 3, and it is clear from fig. 10 that the rolling contact resistant fatigue film has smaller internal stress inside the film after preparation, so that the rolling contact fatigue performance of the film can be further improved.
The invention provides a rolling contact fatigue resistant film on the surface of a gear bearing group, which has good binding force, and by introducing Ti element, on one hand, doped metal atoms form clusters in a DLC film matrix, so that the toughness of the DLC film can be obviously improved, and meanwhile, the internal stress is released through plastic deformation. On the other hand, when a trace amount of Ti is doped, the existence of TiC nano microcrystals can adjust the film structure, improve the hardness and fracture toughness of the DLC film, ensure that the DLC film has excellent tribology performance, and obviously improve the performance of the film in rolling contact.
The invention adopts the combination of multi-arc ion plating and magnetron sputtering technology, and utilizes vacuum vapor deposition technology to deposit Ti-DLC composite film on the surface of the stainless steel substrate. Compared with a single vapor deposition technology, the composite vapor deposition technology is used for depositing the films on the same batch of samples, so that the cleanliness degree of the films in the deposition process can be ensured, and the prepared films are more excellent in performance.
The film provided by the invention has good binding force, ti element is introduced by changing the film preparation mode, so that on one hand, the wear resistance of the film is improved, and on the other hand, the metal-doped DLC film is obtained, and the rolling contact fatigue resistance of the gear bearing group can be improved to a greater extent by taking the Ti-DLC functional layer as an outer layer of the rolling contact fatigue resistance film prepared on the stainless steel surface.
While preferred embodiments of the present invention have been shown and described, various changes and modifications to the embodiments of the present invention will occur to those skilled in the art. Any modification, replacement, improvement, etc. made within the principle and spirit of the embodiments of the present invention should be included in the protection scope of the embodiments of the present invention.
Claims (2)
1. The preparation method of the rolling contact fatigue resistant film on the surface of the gear bearing group is characterized by comprising the following steps of:
s1, carrying out ion etching on the surface of a substrate by adopting a radio frequency ion source in an argon atmosphere, then depositing Cr, and forming a metal Cr bottom layer (1) on the surface of the substrate;
s2, synchronously performing first direct-current magnetron sputtering and multi-arc ion plating deposition on the surface of the metal Cr bottom layer (1) in an argon atmosphere to obtain a CrTi metal transition layer (2);
s3, synchronously performing first direct-current magnetron sputtering and second direct-current magnetron sputtering on the surface of the CrTi metal transition layer (2) in an argon atmosphere to obtain a Ti-C nano transition layer (3);
s4, synchronously performing first direct-current magnetron sputtering and second direct-current magnetron sputtering on the surface of the Ti-C nano transition layer (3) in an argon atmosphere to obtain a Ti-DLC functional layer (4) so as to form a rolling contact fatigue resistant film on the surface of the gear bearing group;
in the step S1, the process parameters for depositing Cr include: bias voltage is 100-400V, pure Cr target arc current is 100A, and time is 25-40 min;
in the step S1, during ion etching, the ion source voltage is set to be 500V, the duty ratio is 50%, the vacuum degree is 0.3-0.7 Pa, the bias voltage is 600-800V, and the etching time is 20-30 min;
in the step S2, the process parameters of synchronous first dc magnetron sputtering and multi-arc ion plating deposition on the surface of the metal Cr bottom layer (1) include: bias voltage is 100V, cr target arc current is 100A, first direct current magnetron sputtering target current is 2.5A, and time is 10-25 min;
in the step S3, the process parameters of the first dc magnetron sputtering and the second dc magnetron sputtering include: bias voltage is 100V, the first direct current magnetron sputtering target current is 2.5A, the second direct current magnetron sputtering target current is 3.0A, and time is 20min;
in the step S4, the technological parameters of performing the first dc magnetron sputtering and the second dc magnetron sputtering synchronously on the surface of the Ti-C nano transition layer (3) include: bias voltage is 100V, the first direct current magnetron sputtering target current is 2.5A, the second direct current magnetron sputtering target current is 3.0-7.0A, and the time is 60-150 min;
in the step S2, the target material deposited by multi-arc ion plating is a metal Cr target; the target material of the first direct current magnetron sputtering in the step S2 and the step S3 is a Ti target; the target material of the second direct current magnetron sputtering in the step S3 is a graphite target;
the metal Cr bottom layer (1) comprises Cr;
the CrTi metal transition layer (2) comprises Cr and Ti, wherein the atomic percentage at% of Cr:72.5%, ti:27.5%;
the Ti-C nano transition layer (3) comprises C and Ti, wherein the C is as follows in atom percent: 81.3%, ti:18.7%;
the Ti-DLC functional layer (4) comprises C and Ti, wherein the C is as follows in atom percent: 55.1 to 98.5 percent of Ti:1.5 to 44.9 percent;
the thickness of the metal Cr bottom layer (1) is 0.3-0.5 mu m;
the thickness of the CrTi metal transition layer (2) is 0.1-0.15 mu m;
the thickness of the Ti-C nano transition layer (3) is 0.05-0.1 mu m;
the Ti-DLC functional layer (4) has a thickness of 1.3 to 2.0 μm.
2. The preparation method of the rolling contact fatigue resistant film on the surface of the gear bearing group according to claim 1, wherein the rolling contact fatigue resistant film on the surface of the gear bearing group prepared by the method comprises a metal Cr bottom layer (1), a CrTi metal transition layer (2), a Ti-C nano transition layer (3) and a Ti-DLC functional layer (4) which are arranged from bottom to top.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444985A (en) * | 2007-12-19 | 2009-06-03 | 中国人民解放军装甲兵工程学院 | Amorphous carbon coating and preparation method and application thereof |
| CN101823353A (en) * | 2010-04-30 | 2010-09-08 | 广州有色金属研究院 | Metal-diamond-like carbon (Me-DLC) nano composite membrane and preparation method thereof |
| JP2013249491A (en) * | 2012-05-30 | 2013-12-12 | Kobe Steel Ltd | Film deposition method |
| CN103920185A (en) * | 2014-04-25 | 2014-07-16 | 湛江师范学院 | Mo metal doped composite diamond-like coating titanium alloy artificial bone joint and manufacturing method thereof |
| CN106868504A (en) * | 2017-01-04 | 2017-06-20 | 兰州空间技术物理研究所 | A kind of Diesel engine piece surface multi-layer wear-resistant antifriction film and preparation method thereof |
| CN107022761A (en) * | 2017-04-28 | 2017-08-08 | 星弧涂层新材料科技（苏州）股份有限公司 | Composite thick film and its film plating process based on DLC film |
| CN107400873A (en) * | 2017-07-26 | 2017-11-28 | 森科五金(深圳)有限公司 | A kind of DLC film and preparation method thereof |
| CN109898064A (en) * | 2019-03-29 | 2019-06-18 | 中南大学 | A kind of DLC/Me-C laminated film and preparation method thereof |
| CN111334794A (en) * | 2020-03-09 | 2020-06-26 | 中国科学院海洋研究所 | Modified film containing Ti transition layer and titanium-doped diamond-like carbon deposited on surface of substrate and method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102216487B (en) * | 2008-10-29 | 2014-07-02 | Ntn株式会社 | Hard multilayer film formed body and method for manufacturing same |
-
2022
- 2022-10-26 CN CN202211318458.2A patent/CN115466924B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444985A (en) * | 2007-12-19 | 2009-06-03 | 中国人民解放军装甲兵工程学院 | Amorphous carbon coating and preparation method and application thereof |
| CN101823353A (en) * | 2010-04-30 | 2010-09-08 | 广州有色金属研究院 | Metal-diamond-like carbon (Me-DLC) nano composite membrane and preparation method thereof |
| JP2013249491A (en) * | 2012-05-30 | 2013-12-12 | Kobe Steel Ltd | Film deposition method |
| CN103920185A (en) * | 2014-04-25 | 2014-07-16 | 湛江师范学院 | Mo metal doped composite diamond-like coating titanium alloy artificial bone joint and manufacturing method thereof |
| CN106868504A (en) * | 2017-01-04 | 2017-06-20 | 兰州空间技术物理研究所 | A kind of Diesel engine piece surface multi-layer wear-resistant antifriction film and preparation method thereof |
| CN107022761A (en) * | 2017-04-28 | 2017-08-08 | 星弧涂层新材料科技（苏州）股份有限公司 | Composite thick film and its film plating process based on DLC film |
| CN107400873A (en) * | 2017-07-26 | 2017-11-28 | 森科五金(深圳)有限公司 | A kind of DLC film and preparation method thereof |
| CN109898064A (en) * | 2019-03-29 | 2019-06-18 | 中南大学 | A kind of DLC/Me-C laminated film and preparation method thereof |
| CN111334794A (en) * | 2020-03-09 | 2020-06-26 | 中国科学院海洋研究所 | Modified film containing Ti transition layer and titanium-doped diamond-like carbon deposited on surface of substrate and method |
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