CN110578110B - Sulfide-based composite film layer, preparation method thereof and wear-resistant workpiece - Google Patents
Sulfide-based composite film layer, preparation method thereof and wear-resistant workpiece Download PDFInfo
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- 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
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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
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- 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
- C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
- C23C14/025—Metallic sublayers
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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
- C23C14/0623—Sulfides, selenides or tellurides
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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
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—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
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Abstract
The invention relates to a sulfide-based composite film layer, a preparation method thereof and a wear-resistant workpiece, and belongs to the field of preparation of inorganic lubricating films. The sulfide-based composite film layer consists of a sulfide matrix and Nd and Cr doped in the sulfide matrix; wherein, the mass percent of Nd is 2-15%, and the mass percent of Cr is 2-16%; the sulfide matrix is molybdenum disulfide or tungsten disulfide. The sulfide-based composite film layer provided by the invention can improve the crystallization strength of a sulfide matrix and improve the structure of the film layer, so that the mechanical properties such as hardness, elastic modulus and the like of the composite film layer are improved, and the friction properties such as friction coefficient, wear resistance and the like are also obviously improved.
Description
Technical Field
The invention belongs to the field of preparation of inorganic lubricating films, and particularly relates to a sulfide-based composite film layer, a preparation method thereof and a wear-resistant workpiece.
Background
In the field of surface engineering, sulfide thin film materials represented by tungsten disulfide and molybdenum disulfide have wide application prospects in the fields of mechanical transmission, photoelectron, biomedicine and the like due to excellent lubricating property, higher oxidation resistance temperature and good antifriction and radiation resistance.
The pure sulfide film has high porosity and low hardness and film base binding force, and the application of the pure sulfide film in high bearing capacity occasions is influenced. High-bearing low-friction MoS prepared by magnetron sputtering deposition in Guanyan and the like2The result of the/Ti composite film (report of tribology, volume 35, phase 3, 5 months in 2015) shows that after the molybdenum disulfide film is doped with Ti element, the friction performance and the mechanical performance of the film are improved, the hardness can reach 12.5Gpa, the friction coefficient is between 0.02 and 0.03, but the wear rate is higher, and the wear resistance is still to be improved.
Disclosure of Invention
The invention aims to provide a sulfide-based composite film layer, so that the problem of poor wear resistance of the conventional sulfide film is solved.
The second objective of the present invention is to provide a method for preparing a sulfide-based composite film layer, so as to solve the problem that the service life of the existing wear-resistant workpiece needs to be further improved.
The third purpose of the present invention is to provide a wear-resistant workpiece, so as to solve the problem that the film bonding force of the wear-resistant working layer of the existing wear-resistant workpiece needs to be further improved.
In order to achieve the purpose, the technical scheme of the sulfide-based composite film layer is as follows:
a sulfide-based composite film layer consists of a sulfide matrix and Nd and Cr doped in the sulfide matrix; wherein, the mass percent of Nd is 2-15%, and the mass percent of Cr is 2-16%; the sulfide matrix is molybdenum disulfide or tungsten disulfide.
Taking molybdenum disulfide as an example, MoS2Has hexagonal crystal layer structure with strong chemical bond in the layerThe layers are bonded by weak van der Waals force, and the special layered structure is MoS2Providing good self-lubricating properties. However, the molybdenum and sulfur atoms at the edge of the layer can not form a complete bond to form a dangling bond, and the dangling bond has certain chemical activity, and is easily oxidized in the friction process under the atmosphere and oxygen-rich environment, so that the friction performance of the dangling bond is sharply reduced, and then the lubrication effect is lost, which seriously affects the engineering application of the dangling bond in the atmosphere environment. In the aspect of film layer structure, a large number of holes are formed in the pure molybdenum disulfide film due to the existence of a plurality of columnar crystals during film forming, so that the mechanical property of the film is poor, and the wear resistance of the film is further influenced.
According to the sulfide-based composite film layer provided by the invention, rare earth element Nd and metal element Cr are utilized to carry out binary co-doping on a sulfide matrix, Cr is used as an alloy element of molybdenum (or tungsten), Nd is used as an active reaction element of S and a micro alloy element of molybdenum (or tungsten), and molybdenum (or tungsten) and S which are not bonded at the edges can be combined, so that the existence of dangling bonds of a pure molybdenum disulfide (or tungsten) film is reduced, and the problem of easiness in oxidation of the pure molybdenum disulfide (or tungsten) film is solved. On the other hand, Nd and Cr atoms with larger and smaller atomic radii are doped into the film structure in a mixed mode, so that the formation of columnar crystals can be effectively inhibited, and the compactness of the inner structure is improved, thereby obviously improving the mechanical property and the wear resistance of the film.
The sulfide-based composite film layer can improve the crystallization strength of a sulfide matrix and improve the structure of the film layer, so that the mechanical properties such as hardness, elastic modulus and the like of the composite film layer are improved, and the friction properties such as friction coefficient, wear resistance and the like are also obviously improved.
In order to further optimize the wear resistance of the sulfide matrix, the sulfide matrix is preferably tungsten disulfide, and in the sulfide matrix composite film layer, the mass percentage of Nd is 5.97-13.71%, and the mass percentage of Cr is 4.69-13.28%.
Aiming at the situation that the sulfide matrix is molybdenum disulfide, in order to further optimize the wear resistance of the film, the sulfide matrix is preferably molybdenum disulfide, and in the sulfide-based composite film layer, the mass percentage of Nd is 6.38-13.95%, and the mass percentage of Cr is 5.13-13.85%.
The preparation method of the sulfide-based composite film adopts the technical scheme that:
a preparation method of a sulfide-based composite film layer comprises the following steps: and (3) mounting a target material in the magnetron sputtering equipment, and performing magnetron sputtering coating on the pretreated substrate to obtain the target material.
According to the preparation method of the sulfide-based composite film layer, the film is prepared in a sputtering deposition mode, so that the binding force between the sulfide-based composite film layer and a workpiece substrate is improved; the method is simple to operate, low in cost and convenient to popularize and apply.
In order to further optimize the sputtering effect of the sulfide-based composite film layer, preferably, the target material comprises a sulfide target material and an Nd-Cr alloy target material, the sulfide target material and the Nd-Cr alloy target material are co-sputtered during magnetron sputtering coating, the working pressure is 0.8-1.8Pa, the sputtering power of the Nd-Cr alloy target material is 5-50W, the sputtering power of the sulfide target material is 150-250W, and the co-sputtering time is 120-150 min. The flow rate of the working gas introduced may be set to 20-100 sccm. The working gas can be conventional gas such as argon.
In order to improve the adhesion of the sulfide-based composite film layer on the substrate, preferably, the pretreated substrate comprises a substrate and a transition layer arranged on the substrate, wherein the transition layer is an Nd-Cr alloy layer, and the Nd-Cr alloy layer is composed of the following components in atomic percentage: nd 5-50%, and Cr in balance.
In order to improve the sputtering effect of the transition layer, preferably, the target material used for plating the transition layer is an Nd-Cr alloy target material, the working pressure during plating is 0.8-1.8Pa, the sputtering power of the Nd-Cr alloy target material is 5-50W, and the sputtering time is 10-20 min.
The technical scheme of the wear-resistant workpiece is as follows:
the wear-resistant workpiece comprises a workpiece base body and a wear-resistant working layer arranged on the workpiece base body, wherein the wear-resistant working layer comprises the sulfide-based composite film layer.
According to the wear-resistant workpiece provided by the invention, the transition layer and the sulfide-based composite film layer are arranged on the workpiece substrate, so that the binding force between the sulfide-based composite film layer and the substrate is improved, the crystal structure of the film layer is improved, the comprehensive performances of the film layer such as thermal stability, wear resistance and the like are obviously improved, and the service life of the related workpiece can be obviously prolonged.
In order to further improve the bonding force between the composite film layer and the substrate, preferably, the wear-resistant working layer further comprises a transition layer arranged between the workpiece substrate and the sulfide-based composite film layer, and the transition layer is an Nd-Cr alloy layer. The thickness of the Nd-Cr alloy layer may be set to 0.1 to 0.3. mu.m.
In order to further optimize the film binding force and the tribological characteristics of the workpiece, the thickness of the sulfide-based composite film layer is preferably 2-4 μm.
Detailed Description
The following examples are provided to further illustrate the practice of the invention.
First, the embodiment of the sulfide-based composite film layer of the present invention
Example 1
The sulfide-based composite film layer of the embodiment is composed of a tungsten disulfide matrix and Nd and Cr doped in the tungsten disulfide matrix; wherein, the mass percent of Nd is 13.71%, the mass percent of Cr is 4.69%, and the sum of the mass percent of Nd, Cr and tungsten disulfide is 100%.
Examples 2 to 20
The sulfide-based composite film layers of examples 2 to 20 were composed of a tungsten disulfide matrix and Nd and Cr doped in the tungsten disulfide matrix; the contents of the ingredients are listed in table 1.
TABLE 1 compositional makeup of sulfide-based (tungsten disulfide) composite film layers of examples 2-20
Example 21
The sulfide-based composite film layer of the embodiment is composed of a molybdenum disulfide matrix and Nd and Cr doped in the molybdenum disulfide matrix; wherein, the mass percent of Nd is 13.95%, the mass percent of Cr is 5.13%, and the sum of the mass percent of Nd, Cr and molybdenum disulfide is 100%.
Examples 22 to 34
The sulfide-based composite film layers of examples 22 to 34 were composed of a molybdenum disulfide matrix and Nd and Cr doped in the molybdenum disulfide matrix; the contents of the ingredients are listed in table 2.
TABLE 2 compositional makeup of sulfide-based (molybdenum disulfide) composite film layers of examples 22-34
Second, the following specific examples of the method for producing a sulfide-based composite film layer will be described with respect to the production of the sulfide-based composite film layers of examples 1 to 34.
Example 35
The method for preparing a sulfide-based composite film layer according to this embodiment will be described with reference to example 1, and specifically includes the following steps:
1) in an ultrasonic cleaner, sequentially using absolute ethyl alcohol and acetone to carry out ultrasonic cleaning on a stainless steel substrate; loading the cleaned ultrasonic substrate into a vacuum chamber of a magnetron sputtering device, and vacuumizing the vacuum chamber to 5 x 10-3Pa, introducing working gas argon, controlling the flow of the argon to be 40sccm and the working pressure to be 1.2Pa, and heating the stainless steel substrate for 90min to 300 ℃.
2) Under the working pressure, a 20W direct current power supply is used for exciting an Nd-Cr alloy target material (the atomic percentage composition is as follows: nd: 50%, Cr: 50 percent) to form stable glow, and plating the surface of the substrate for 20min to form a Nd-Cr alloy layer with the thickness of 0.2 mu m on the surface; however, the device is not suitable for use in a kitchenPost-open WS2A target power supply for co-sputtering with the Nd-Cr alloy target with a sputtering power of 20W, WS2The sputtering power of the target is 120W, the co-sputtering time is 120min, and then the Nd-Cr/WS with the thickness of 3 mu m can be obtained by natural cooling2And (3) compounding the film.
Examples 36 to 38
The sulfide-based composite film layers of examples 36 to 38 were prepared in the same manner as in example 35 except that the operating pressures were 0.4Pa, 0.8Pa and 1.6Pa, respectively.
Examples 39 to 42
The sulfide-based composite film layers of examples 39 to 42 were prepared in substantially the same manner as in example 35, except that the sputtering powers of the Nd — Cr alloy targets were 10W, 30W, 40W, and 50W, respectively.
Examples 43 to 46
The sulfide-based composite film layers of examples 43 to 46 were prepared in substantially the same manner as in example 35, except that the flow rates of argon gas were 20sccm, 60sccm, 80sccm, and 100sccm, respectively.
Examples 47 to 50
The sulfide-based composite film layers of examples 47 to 50 were prepared in the same manner as in example 35, except that the Nd — Cr alloy target had the following atomic percentage composition: nd: 10%, Cr: 90 percent; the working pressure is 0.4Pa, 0.8Pa, 1.2Pa and 1.6Pa respectively.
Examples 51 to 54
The sulfide-based composite film layers of examples 51 to 54 were prepared in the same manner as in example 35, except that the Nd — Cr alloy target had the following atomic percentage composition: nd: 5%, Cr: 95 percent; the working pressure is 0.4Pa, 0.8Pa, 1.2Pa and 1.6Pa respectively.
Example 55
The method for preparing a sulfide-based composite film layer according to this embodiment will be described with reference to the preparation of the sulfide-based composite film layer according to embodiment 21, and specifically includes the following steps:
1) in an ultrasonic cleaner, sequentially using absolute ethyl alcohol and acetone to carry out ultrasonic cleaning on a stainless steel substrate; loading the cleaned ultrasonic substrate into a magnetron sputtering deviceIn the vacuum chamber of the injection device, the vacuum chamber is firstly vacuumized to 5 x 10-3Pa, introducing working gas argon, controlling the flow of the argon to be 40sccm and the working pressure to be 1.2Pa, and heating the stainless steel substrate for 90min to 300 ℃.
2) Under the working pressure, a 20W direct current power supply is used for exciting an Nd-Cr alloy target material (the atomic percentage composition is as follows: nd: 50%, Cr: 50 percent) to form stable glow, and plating the surface of the substrate for 20min to form a Nd-Cr alloy layer with the thickness of 0.2 mu m on the surface; then opens the MoS2A target power supply for co-sputtering with the Nd-Cr alloy target with a sputtering power of 20W and MoS2The sputtering power of the target is 120W, the co-sputtering time is 120min, and then Nd-Cr/MoS with the thickness of 3 mu m can be obtained by natural cooling2And (3) compounding the film.
Examples 56 to 58
The sulfide-based composite film layers of examples 56 to 58 were prepared in the same manner as in example 55 except that the operating pressures were 0.4Pa, 0.8Pa and 1.6Pa, respectively.
Examples 59 to 62
The sulfide-based composite film layers of examples 59 to 62 were prepared in substantially the same manner as in example 55, except that the sputtering powers of the Nd — Cr alloy targets were 10W, 30W, 40W, and 50W, respectively.
Examples 63 to 66
The sulfide-based composite film layers of examples 63 to 66 were prepared in substantially the same manner as in example 55 except that the flow rates of argon gas were 20sccm, 60sccm, 80sccm, and 100sccm, respectively.
Example 67
The preparation method of the sulfide-based composite film layer of example 67 is substantially the same as that of example 55, except that the Nd — Cr alloy target material has the following atomic percentage composition: nd: 10%, Cr: 90 percent.
Example 68
The sulfide-based composite film layer of example 68 was prepared in substantially the same manner as in example 55, except that the Nd — Cr alloy target had the following atomic percentage composition: nd: 5%, Cr: 95 percent.
In other embodiments of the method for preparing a sulfide-based composite film, a plasma metal layer can be pre-sputtered for 5 minutes on the workpiece substrate before the transition layer is sputtered to achieve a better bonding effect.
And thirdly, the embodiments of the wear-resistant workpiece respectively correspond to the final products obtained by the preparation methods of the embodiments 35 to 68, and the final products comprise a workpiece substrate, a transition layer plated on the workpiece and a sulfide composite film layer plated on the transition layer.
The workpiece substrate of the embodiment is a stainless steel substrate, and aiming at other implementation situations, the wear-resistant working surface of the workpiece is plated.
Fourth, comparative example
Comparative example 1
This comparative example prepares pure WS2A thin film was produced in substantially the same manner as in example 35 except that only WS was used after the Nd-Cr alloy layer was formed2The target is sputtered, and the specific sputtering parameters are kept consistent.
Comparative example 2
This comparative example prepares pure MoS2A thin film was produced in substantially the same manner as in example 55 except that only MoS was used after the Nd-Cr alloy layer was formed2The target is sputtered, and the specific sputtering parameters are kept consistent.
Fifth, example of experiment
Comparative pure WS of this Experimental example2Thin film, pure MoS2The binding force, hardness, friction coefficient and wear rate of the film and the corresponding composite film. The binding force and the hardness are obtained according to the test of a nano-indenter, the friction coefficient is obtained according to the test of a high-temperature friction wear testing machine (the friction radius is 4mm, the diameter of a grinding ball is 6mm, the rotating speed is 336r/min, and the load is 1N), and the wear rate is obtained by calculation according to a formula W (V/F) L (in the formula, V is the wear volume of a grinding trace, F is the normal load applied by the friction test, and L is the length of a friction stroke).
Specific detection results are shown in tables 1 and 2.
Table 1 comparison of the properties of the wear resistant layer of comparative example 1 and the typical examples
Table 2 comparison of the properties of the wear resistant layer of comparative example 2 and the typical examples
(in tables 1 and 2, the parameters of the plating films of the experimental examples and the comparative examples were the same, i.e., working pressure was 1.2Pa, sputtering power was 20W, and argon flow rate was 40 sccm.)
As can be seen from the experimental results of tables 1 and 2, by doping the rare earth element Nd and the metal element Cr into the sulfide film, the bonding force, hardness, and frictional wear properties of the film layer are improved, and excellent mechanical properties and wear resistance are exhibited.
Claims (8)
1. A sulfide-based composite film layer is characterized by consisting of a sulfide matrix and Nd and Cr doped in the sulfide matrix;
the sulfide matrix is tungsten disulfide, and in the sulfide-based composite film layer, the mass percentage of Nd is 5.97-13.71%, and the mass percentage of Cr is 4.69-13.28%;
or the sulfide matrix is molybdenum disulfide, and in the sulfide-based composite film layer, the mass percentage of Nd is 6.38-13.95%, and the mass percentage of Cr is 5.13-13.85%;
the preparation method of the sulfide-based composite film layer comprises the following steps: mounting a target material in a magnetron sputtering device, and performing magnetron sputtering coating on the pretreated substrate;
the target comprises a sulfide target and an Nd-Cr alloy target, and the sulfide target and the Nd-Cr alloy target are co-sputtered during magnetron sputtering coating.
2. A method for producing the sulfide-based composite film according to claim 1, comprising the steps of: mounting a target material in a magnetron sputtering device, and performing magnetron sputtering coating on the pretreated substrate;
the target comprises a sulfide target and an Nd-Cr alloy target, and the sulfide target and the Nd-Cr alloy target are co-sputtered during magnetron sputtering coating.
3. The method as claimed in claim 2, wherein the working pressure is 0.8-1.8Pa, the sputtering power of the Nd-Cr alloy target is 5-50W, the sputtering power of the sulfide target is 150-250W, and the co-sputtering time is 120-150 min.
4. The method for preparing the sulfide-based composite film according to claim 2 or 3, wherein the pretreated substrate comprises a substrate and a transition layer disposed on the substrate, wherein the transition layer is an Nd-Cr alloy layer, and the Nd-Cr alloy layer is composed of the following components in atomic percentage: nd 5-50%, and Cr in balance.
5. The method for preparing the sulfide-based composite film according to claim 4, wherein a target material used for plating the transition layer is an Nd-Cr alloy target material, the working pressure during plating is 0.8-1.8Pa, the sputtering power of the Nd-Cr alloy target material is 5-50W, and the sputtering time is 10-20 min.
6. A wear-resistant workpiece comprising a workpiece substrate and a wear-resistant working layer provided on the workpiece substrate, the wear-resistant working layer comprising the sulfide-based composite film layer according to claim 1.
7. The wear resistant workpiece of claim 6, wherein the wear resistant working layer further comprises a transition layer disposed between the workpiece substrate and the sulfide-based composite film layer, the transition layer being an Nd-Cr alloy layer.
8. The wear-resistant workpiece according to claim 6 or 7, wherein the sulfide-based composite film layer has a thickness of 2 to 4 μm.
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