阅读说明：本技术 一种硫化物基复合膜层及其制备方法和耐磨工件 (Sulfide-based composite film layer, preparation method thereof and wear-resistant workpiece ) 是由 蔡海潮 薛玉君 司东宏 李航 贺江涛 马喜强 杨芳 刘春阳 于 2019-10-15 设计创作，主要内容包括：本发明涉及一种硫化物基复合膜层及其制备方法和耐磨工件,属于无机润滑膜的制备领域。该硫化物基复合膜层由硫化物基体和掺杂在硫化物基体中的Nd、Cr组成；其中,Nd的质量百分含量为2-15％,Cr的质量百分含量为2-16％；所述硫化物基体为二硫化钼或二硫化钨。本发明提供的硫化物基复合膜层,可提高硫化物基体的结晶强度,改善膜层结构,从而使复合膜层的硬度、弹性模量等力学性能得以提高,摩擦系数、耐磨性等摩擦学性能也得到显著改善。(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.)

1. A sulfide-based composite film layer is characterized by consisting 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.

2. The sulfide-based composite film according to claim 1, wherein the sulfide matrix is tungsten disulfide, and in the sulfide-based composite film, the mass percentage of Nd is 5.97 to 13.71%, and the mass percentage of Cr is 4.69 to 13.28%.

3. The sulfide-based composite film according to claim 1, wherein the sulfide matrix is molybdenum disulfide, and in the sulfide-based composite film, the mass percentage of Nd is 6.38-13.95%, and the mass percentage of Cr is 5.13-13.85%.

4. a method for producing the sulfide-based composite film layer according to any one of claims 1 to 3, comprising the steps of: 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.

5. The method for preparing the sulfide-based composite film according to claim 4, wherein the target comprises a sulfide target and an Nd-Cr alloy target, the sulfide target and the Nd-Cr alloy target co-sputter during magnetron sputtering coating, 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-.

6. The method for preparing the sulfide-based composite film according to claim 4 or 5, 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.

7. The method for preparing the sulfide-based composite film according to claim 6, 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.

8. 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 any one of claims 1 to 3.

9. the wear resistant article of claim 8 wherein the wear resistant working layer further comprises a transition layer disposed between the article substrate and the sulfide-based composite film layer, the transition layer being an Nd-Cr alloy layer.

10. The wear-resistant workpiece according to claim 8 or 9, wherein the sulfide-based composite film layer has a thickness of 2 to 4 μm.

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, strong chemical bonds in the layers, and weak van der Waals force between the layers, and the special layer 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