US 12,291,772 B2
Low-friction long-life ultra-lattice composite coating as well as preparation method and use thereof
Jibin Pu, Ningbo (CN); Yanbin Shi, Ningbo (CN); and Haixin Wang, Ningbo (CN)
Assigned to NINGBO INSTITUTE OF MATERIALS TECHNOLOGY AND ENGINEERING, CHINESE ACADEMY OF SCIENCES, Ningbo (CN)
Appl. No. 18/833,935
Filed by NINGBO INSTITUTE OF MATERIALS TECHNOLOGY AND ENGINEERING, CHINESE ACADEMY OF SCIENCES, Ningbo (CN)
PCT Filed Dec. 11, 2023, PCT No. PCT/CN2023/137948
§ 371(c)(1), (2) Date Jul. 29, 2024,
PCT Pub. No. WO2024/244380, PCT Pub. Date Dec. 5, 2024.
Claims priority of application No. 202310611417.0 (CN), filed on May 29, 2023.
Prior Publication US 2025/0109485 A1, Apr. 3, 2025
Int. Cl. C23C 14/35 (2006.01); C23C 14/02 (2006.01); C23C 14/06 (2006.01)
CPC C23C 14/35 (2013.01) [C23C 14/022 (2013.01); C23C 14/0623 (2013.01); C23C 14/0641 (2013.01)] 20 Claims
OG exemplary drawing
 
1. A preparation method of a low-friction long-life ultra-lattice composite coating, comprising:
by using an unbalanced magnetron sputtering technology based on a titanium target as a negative electrode target and an inert gas as a working gas, applying a sputtering current to the titanium target, and applying a back bias voltage to a matrix, thereby depositing a titanium transition layer on a surface of the matrix, wherein the sputtering current is 3.0 A-5.0 A, the back bias voltage of the matrix is −100 V to −150 V, a flow of the working gas is 20 sccm-30 sccm, a temperature of the matrix is 50° C.-150° C., a pressure of a reaction cavity is 0.1 Pa-2.0 Pa, and a deposition time is 300 s-900 s;
by using the unbalanced magnetron sputtering technology based on the titanium target as the negative electrode target and the inert gas and N2 as the working gas, applying the sputtering current to the titanium target, and applying the back bias voltage to the matrix, thereby depositing a TiNx bearing layer on a surface of the titanium transition layer, wherein the sputtering current is 3.0 A-5.0 A, the back bias voltage of the matrix is −100 V to −150 V, a flow of the inert gas is 20 sccm-30 sccm, a flow of the N2 is 5 sccm-15 sccm, the temperature of the matrix is 50° C.-150° C., the pressure of the reaction cavity is 0.1 Pa-2.0 Pa, and the deposition time is 2400 s-4800 s;
by using the unbalanced magnetron sputtering technology based on the titanium target and a molybdenum disulfide target as electrode targets and the inert gas and the N2 as the working gas, applying the sputtering current to the titanium target and the molybdenum disulfide target, and applying the back bias voltage to the matrix, thereby depositing a TiNx/MoS2 gradient transition layer on a surface of the TiNx bearing layer, wherein the sputtering current applied to the titanium target gradually decreases from 3.0 A-5.0 A to 0, the sputtering current applied to the molybdenum disulfide target gradually increases from 0 to 1.2 A-2.0 A, the back bias voltage of the matrix is −30 V to −70 V, the flow of the inert gas is 10 sccm-20 sccm, the flow of the N2 is 5 sccm-15 sccm, the temperature of the matrix is 50° C.-150° C., the pressure of the reaction cavity is 0.1 Pa-2.0 Pa, and the deposition time is 300 s-900 s;
by using the unbalanced magnetron sputtering technology based on a metal Me target and the molybdenum disulfide target as the electrode targets and the inert gas as the working gas, applying the sputtering current to the metal Me target and the molybdenum disulfide target, and applying the back bias voltage to the matrix, thereby depositing a MoS2/Me gradient transition layer on a surface of the TiNx/MoS2 gradient transition layer, wherein the sputtering current applied to the metal Me target gradually increases from 0 to 0.6 A-1.4 A, the sputtering current applied to the molybdenum disulfide target is 1.2 A-2.0 A, the back bias voltage of the matrix is −30 V to −70 V, the flow of the inert gas is 10 sccm-20 sccm, the temperature of the matrix is 50° C.-150° C., the pressure of the reaction cavity is 0.1 Pa-2.0 Pa, and the deposition time is 300 s-900 s;
and, by using the unbalanced magnetron sputtering technology based on the molybdenum disulfide target and the metal Me target as the electrode targets and the inert gas as the working gas, applying the back bias voltage to the matrix, applying the sputtering current to the molybdenum disulfide target and the metal Me target, and alternately depositing a MoS2 layer and a Me layer, thereby depositing a MoS2/Me ultra-lattice layer on a surface of the MoS2/Me gradient transition layer, so as to obtain the low-friction long-life ultra-lattice composite coating, wherein the sputtering current applied to the molybdenum disulfide target is 1.2 A-2.0 A, the sputtering current applied to the metal Me target is 0.6 A-1.4 A, the back bias voltage of the matrix is −30 V to −70 V, a flow of the working gas is 10 sccm-20 sccm, the temperature of the matrix is 50° C.-150° C., the pressure of the reaction cavity is 0.1 Pa-2.0 Pa, and the deposition time is 6000 s-8000 s; the deposition time for alternately depositing the MoS2 layer and the Me layer in each period is 10 s-90 s;
the low-friction long-life ultra-lattice composite coating comprising: the titanium transition layer, the TiNx bearing layer, the TiNx/MoS2 gradient transition layer, the MoS2/Me gradient transition layer, and the MoS2/Me ultra-lattice layer which are successively formed on the surface of the matrix; wherein, x is 0.5-1, Me is selected from a combination of any one or more than two of Ti, Zr, V, Nb, Cr, Mo, and Cd; furthermore, in a direction gradually far away from the matrix, a content of MoS2 in the TiNx/MoS2 gradient transition layer is increasing, and a content of MoS2 in the MoS2/Me gradient transition layer is decreasing; the MoS2/Me ultra-lattice layer comprises a plurality of alternately stacked periodic layers, and each alternately stacked periodic layer comprises one MoS2 layer and one Me layer; the MoS2 layer in the MoS2/Me ultra-lattice layer is oriented and grows parallel to a MoS2 (002) plane; a friction coefficient of the low-friction long-life ultra-lattice composite coating in a vacuum environment is less than 0.02, and a wear life of the low-friction long-life ultra-lattice composite coating is more than 4×106 revolutions.