CN112992425B - Preparation method of copper-based composite electric contact material with gradient structure - Google Patents
Preparation method of copper-based composite electric contact material with gradient structure Download PDFInfo
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Abstract
The invention discloses a preparation method of a copper-based composite electric contact material with a gradient structure, which comprises the steps of pretreatment of a substrate, sputtering copper plating treatment, reactive co-sputtering treatment and the like. The invention prepares the Cu/TiN-Ni-Cu-Re composite coating on the QTi3.5 surface by a magnetron sputtering method, and combines the TiN coating with good chemical stability and conductivity and the Ni-Cu-Re particles with good self-lubricating property to obtain the wear-resistant composite coating with controllable thickness and good conductivity, and simultaneously reserves the excellent performance of the QTi3.5 substrate, and effectively slows down the interface stress between different coatings by preparing the pure copper transition coating, improves the binding force between the coating and the substrate and between different coatings, and obtains the electric contact material with good comprehensive performance, thereby prolonging the service life of the electric contact material.
Description
Technical Field
The invention relates to a gradient composite coating material, in particular to a preparation method of a copper-based composite electric contact material with a gradient structure.
Background
The electric contact material is often used under the interaction of electricity, heat, force and different environments, and due to different contact loads, different contact forms and different use environments, when the performance is insufficient, the problem of electric contact failure is easy to occur, so that a major accident or disaster is caused, and a high requirement is put forward on the use reliability of the electric contact material.
Titanium bronze is a copper alloy made of pure copper with the addition of titanium and the like, and the material has high strength, high hardness, excellent wear resistance, fatigue resistance, corrosion resistance and heat resistance. The titanium bronze has the advantages of no spark generation during impact, no magnetism and high elastic limit, and can be used for manufacturing various elements with high strength, high elasticity and high wear resistance. On the other hand, the titanium element is widely distributed, the content of the titanium element exceeds 0.4 percent of the crust quality, and the part prepared by adopting the titanium bronze can replace Cu-Be alloy in the field of high strength and high elasticity, thereby improving the labor environment, saving the use of beryllium cobalt strategic resources and creating economic benefits for society and enterprises. The prior methods for preparing conductive elastic components such as titanium copper alloy wires, titanium copper alloy rods and titanium copper alloy belts describe a process for obtaining high-conductivity and high-elasticity components by using different raw materials and combining vacuum smelting and plastic deformation processing with a subsequent heat treatment process.
Titanium nitride is a material with many excellent properties, such as low coefficient of friction, high hardness (coating hardness up to 2200HV), good corrosion and wear resistance, and good thermal and electrical conductivity. On the other hand, titanium nitride has better chemical stability, generally does not react with water, water vapor, hydrochloric acid, sulfuric acid and the like, and can be stably used in a fretting contact corrosion environment. According to the research results of the predecessors, the Ni-Cu-Re alloy can generate a self-generated lubricating film during friction so as to play a role in lubricating and reducing friction, and the Ni-Cu-Re alloy containing Re and Cu forms a compound containing Re and Cu during friction, so that the Ni-Cu-Re alloy has the performance characteristics of low melting point, small hardness and easiness in shearing. In the friction process, a lubricating interface film formed by a compound containing Re and Cu exists at the friction interface, so that the friction coefficient is maintained at a lower value, and the formation and the loss of the lubricating film belong to dynamic processes, have a self-repairing function and effectively slow down the loss of materials in the friction environment.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a copper-based composite electric contact material with a gradient structure, which comprises the following steps:
(1) carrying out mechanical polishing treatment on the QTi3.5 matrix and sequentially carrying out ultrasonic cleaning in an acetone solution and an absolute ethyl alcohol solution;
(2) placing the QTi3.5 matrix pretreated in the step (1) on the top of a closed vacuum cavity, placing zirconia balls at the bottom of the closed vacuum cavity, and mechanically grinding the QTi3.5 matrix;
(3) putting the QTi3.5 matrix treated in the step (2) into an acetone solution for ultrasonic cleaning, and then putting the cleaned matrix into a mixed acid solution for cleaning;
(4) clamping the QTi3.5 matrix processed in the step (3) on a sample table of a magnetron co-sputtering system, and adjusting the included angles and the distances between the center of the QTi3.5 matrix and the centers of the surfaces of an industrial pure titanium TA1 target, an industrial pure copper T1 target and a Ni-Cu-Re target to be equal;
(5) a three-target magnetron sputtering system is adopted, a sputtering chamber is vacuumized, a heating power supply is turned on to heat a sample platform to start heating, a control valve is turned on to fill argon, a copper target direct current power supply is turned on to carry out sputtering treatment on a copper target with the purity not lower than 99.95 wt%, and a pure copper transition coating is formed on the surface of a QTi3.5 matrix;
(6) closing an industrial pure copper T1 target direct-current power supply and an upper baffle, closing a QTi3.5 substrate sample table baffle device, opening an industrial pure titanium TA1 target and an upper baffle of a Ni-Cu-Re target, adjusting argon pressure, opening an industrial pure titanium TA1 target radio-frequency power supply and a Ni-Cu-Re target radio-frequency power supply, adjusting the power of an industrial pure titanium TA1 target radio-frequency power supply and the power of a Ni-Cu-Re target radio-frequency power supply, carrying out sputtering cleaning, opening a valve, filling nitrogen, opening a QTi3.5 substrate sample table baffle device, adjusting the power of the industrial pure titanium TA1 target radio-frequency power supply and the power of the Ni-Cu-Re target radio-frequency power supply, carrying out reactive co-sputtering, and preparing the QTi3.5/Cu/TiN-Cu-Re composite coating;
(7) and (5) placing the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating prepared in the step (6) in a vacuum furnace for annealing treatment to obtain the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating.
The method can prepare the copper-based composite electric contact material with excellent performance by accurately controlling the process parameters, and specifically controls the process parameters such as time, temperature, size, efficiency and the like as follows:
in the step (1), ultrasonic cleaning is carried out in an acetone solution for 10-15min, and ultrasonic cleaning is carried out in an absolute ethyl alcohol solution for 5-10 min; in the step (2), the surface mechanical grinding treatment time is 20-60 min; in the step (3), the QTi3.5 matrix is ultrasonically cleaned in an acetone solution for 10-15min and in a mixed acid solution for 5-10s, and the mass ratio of the mixed acid cleaning solution is H 2 SO 4 :HNO 3 The ultrapure water is 5:3: 2; in the step (5), the sputtering treatment time is 3-5 min; in the step (6), the sputtering cleaning time is 8-15min, and the reaction co-sputtering time is 40-80 min; in the step (7), the annealing time is 90-150 min.
In the step (2), the number of the zirconia balls is 180-220, and the diameter of the zirconia balls is 4-6 mm; in the step (4), the included angle is 50-75 degrees, and the distance is 60-90 mm.
In the step (5), the temperature is raised to 100-150 ℃; in the step (7), the annealing temperature is 300-.
In the step (2), the vibration frequency of the mechanical grinding treatment is 40-60 Hz; in the step (5), the power of the direct current power supply of the copper target is 150-200W; in the step (6), during sputtering cleaning, the RF power of the industrial pure titanium TA1 target is 150-250W, the RF power of the Ni-Cu-Re target is 120-160W, during reactive co-sputtering, the RF power of the industrial pure titanium TA1 target is 180-250W, and the RF power of the Ni-Cu-Re target is 140-180W.
In the step (5), the vacuum degree of the sputtering chamber is less than or equal to 6 multiplied by 10 -3 Pa, argon pressure is 3-5 Pa; in the step (6), the argon pressure is 0.5-1.8Pa, and the nitrogen flow is 20-50 sccm; in the step (7), the vacuum degree of the vacuum furnace is less than or equal to 3 multiplied by 10 -2 Pa。
The invention has the beneficial effects that:
(1) according to the invention, the surface residual compressive stress is generated by processing the QTi3.5 matrix through surface mechanical grinding, the surface layer crystal grains are refined, and then a pure copper transition layer is prepared through magnetron sputtering, so that the difference of thermal expansion coefficients and the residual stress between different interface layers are reduced, and the diffusion bonding between the interface layers is promoted, thereby improving the bonding force between the Cu/TiN-Ni-Cu-Re composite coating and the QTi3.5 base material; (2) the Cu/TiN-Ni-Cu-Re gradient composite coating is prepared on the surface of the QTi3.5 matrix by a magnetron reaction co-sputtering method, the TiN coating has high hardness, good chemical stability and excellent wear resistance, and Ni-Cu-Re particles form a boundary lubricating film in a friction state, so that the friction coefficient is reduced, and the composite coating has a self-lubricating effect. After annealing treatment, Ni-Cu-Re particles are uniformly distributed in the TiN coating, so that a large number of interfaces are increased, columnar crystal gaps of the TiN are filled, the oxidation resistance and toughness of the TiN coating are improved, and the comprehensive performance of the composite coating is improved; (3) the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating prepared by the invention has good oxidation resistance and antifriction wear resistance, has stable performance under long-time work, can realize artificial regulation of the thickness of the coating, and can meet the use requirements under the condition of working condition change.
Drawings
FIG. 1 is the scanning electron microscope image of the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating obtained in example 1.
FIG. 2 is a scanning electron microscope photograph of the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating obtained in example 1 after friction and wear.
FIG. 3 is the scanning electron microscope image of the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating obtained in example 2.
FIG. 4 is a scanning electron micrograph of the QTi3.5 matrix obtained in comparative example 1 after frictional wear.
Detailed Description
The present invention is described below with reference to examples, which are provided for illustration only and are not intended to limit the scope of the present invention.
Example 1
A preparation method of a copper-based composite electric contact material with a gradient structure comprises the following steps: selecting a QTi3.5 matrix (Ti3.5-4.0 wt%, total impurity content less than or equal to 0.5% and Cu in balance) of copper alloy, carrying out mechanical polishing treatment on the QTi3.5 matrix, carrying out ultrasonic cleaning in an acetone solution for 10min, carrying out ultrasonic cleaning in an absolute ethyl alcohol solution for 10min, placing the pretreated QTi3.5 matrix on the top of a closed cavity for mechanical grinding treatment, and carrying out bottom grinding treatment on the matrixThe number of the zirconia balls placed in the groove is 180, the diameter of each steel ball is 4mm, the processing time is 30min, the vibration frequency is 45Hz, the QTi3.5 matrix after mechanical grinding is placed in an acetone solution for ultrasonic cleaning for 10min, the matrix is cleaned in a mixed acid solution for 5s, and the mass ratio of the mixed acid solution is H 2 SO 4 :HNO 3 The ultrapure water is 5:3: 2; clamping the processed QTi3.5 matrix on a sample table of a reaction magnetron co-sputtering system, adjusting the included angle of the center of the QTi3.5 matrix and the centers of an industrial pure titanium TA1 target, an industrial pure copper T1 target and a Ni-Cu-Re target to 65 degrees and the distance to 72mm, and pumping the vacuum degree of a magnetron sputtering chamber to 1 multiplied by 10 -3 Pa, turning on a heating power supply to increase the temperature of a sample table to 110 ℃, filling high-purity argon and adjusting the air pressure to 3.2Pa, setting the power of a direct-current power supply of an industrial pure copper T1 target to 160W, closing an industrial pure titanium TA1 target and a Ni-Cu-Re target baffle, opening an industrial pure copper T1 target baffle, sputtering the industrial pure copper T1 target for 5min, closing the copper target baffle and a QTi3.5 matrix sample table baffle device, opening the industrial pure titanium TA1 target and the Ni-Cu-Re target baffle, respectively setting the power of radio frequency power supplies to 160W and 140W, sputtering and cleaning for 10min, filling nitrogen, adjusting the gas flow to 35sccm, opening the QTi3.5 matrix sample table baffle device, setting the power of the industrial pure titanium TA1 target sample to 200W, setting the power of the Ni-Cu-Re target to 160W, sputtering for 60min, putting the prepared QTi3.5/Cu/TiN-Ni-Cu-Re composite coating in a vacuum furnace for gradient annealing, vacuum degree of 1X 10 -2 Pa, the annealing temperature is set to be 400 ℃, and the annealing time is 90 min.
The QTi3.5 surface is a gradient composite structure layer consisting of a pure Cu transition layer and TiN-Ni-Cu-Re, gaps are not left between columnar crystals, the structure is compact, the transition pure copper layer is well combined with the upper TiN-Ni-Cu-Re composite layer and the lower QTi3.5 base material without cracking, and the thicknesses of the transition layer and the composite layer are about 1.5 mu m. The surface TiN-Ni-Cu-Re composite layer, the pure copper transition layer, the QTi3.5 surface fine grain layer and the QTi3.5 coarse grain matrix are arranged from the surface to the core of the matrix in sequence.
Adopting a multifunctional friction and wear instrument, wherein the friction condition is dry friction, the wear mode is unidirectional circular sliding, a friction pair is a 4mm G10 steel ball, under the load of 5N, the linear velocity is 10mm/s, the total movement distance is 18m, the average friction coefficient is measured to be 0.35,the wear rate is 0.33mm 3 /(N·m)。
Example 2
A preparation method of a copper-based composite electric contact material with a gradient structure adopts the same raw materials and preparation process as those in example 1, and changes the sputtering time of an industrial pure titanium TA1 target radio frequency power supply and a Ni-Cu-Re target radio frequency power supply during working to 100 min; the gradient composite coating was analyzed in cross section and had a thickness of 3 μm.
Adopting a multifunctional friction and wear instrument, wherein the friction condition is dry friction, the wear mode is one-way circular sliding, the friction pair is a 4mm G10 steel ball, under the 5N load, the linear speed is 10mm/s, the total movement distance is 18m, the measured average friction coefficient is 0.37, and the wear rate is 0.42mm 3 /(N·m)。
Comparative example 1
A QTi3.5 matrix material comprises the following steps: selecting copper alloy with QTi3.5(Ti3.5-4.0 wt%, total impurity less than or equal to 0.5 wt%, and Cu as the rest), ultrasonic cleaning in acetone solution for 10min, and ultrasonic cleaning in absolute ethanol solution for 10 min.
Adopting a multifunctional friction and wear instrument, wherein the friction condition is dry friction, the wear mode is one-way circular sliding, the friction pair is a 4mm G10 steel ball, under the 5N load, the linear speed is 10mm/s, the total movement distance is 18m, the measured average friction coefficient is 0.51, and the wear rate is 1.92mm 3 /(N·m)。
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The preparation method of the copper-based composite electric contact material with the gradient structure is characterized by comprising the following steps of:
(1) carrying out mechanical polishing treatment on the QTi3.5 matrix and sequentially carrying out ultrasonic cleaning in an acetone solution and an absolute ethyl alcohol solution;
(2) placing the QTi3.5 matrix pretreated in the step (1) on the top of a closed vacuum cavity, placing zirconia balls at the bottom of the closed vacuum cavity, and mechanically grinding the QTi3.5 matrix;
(3) putting the QTi3.5 matrix treated in the step (2) into an acetone solution for ultrasonic cleaning, and then putting the cleaned matrix into a mixed acid solution for cleaning;
(4) clamping the QTi3.5 matrix processed in the step (3) on a sample table of a magnetron co-sputtering system, and adjusting the included angles and the distances between the center of the QTi3.5 matrix and the centers of the surfaces of an industrial pure titanium TA1 target, an industrial pure copper T1 target and a Ni-Cu-Re target to be equal;
(5) adopting a three-target magnetron sputtering system, vacuumizing a sputtering chamber, turning on a heating power supply to heat a sample platform, starting to heat, turning on a control valve to fill argon, turning on a copper target direct current power supply to sputter a copper target with the purity not lower than 99.95 wt%, and forming a pure copper transition coating on the surface of a QTi3.5 substrate;
(6) closing a direct-current power supply and an upper baffle of an industrial pure copper T1 target, closing a QTi3.5 substrate sample table baffle device, opening baffles above an industrial pure titanium TA1 target and a Ni-Cu-Re target, adjusting argon pressure, opening a radio-frequency power supply of an industrial pure titanium TA1 target and a radio-frequency power supply of a Ni-Cu-Re target, adjusting the radio-frequency power supply power of an industrial pure titanium TA1 target and the radio-frequency power supply power of a Ni-Cu-Re target, carrying out sputtering cleaning, opening a valve to fill nitrogen, opening a QTi3.5 substrate sample table baffle device, adjusting the radio-frequency power supply power of the industrial pure titanium TA1 target and the radio-frequency power supply power of the Ni-Cu-Re target, carrying out reactive co-sputtering, and preparing a QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating;
(7) and (4) placing the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating prepared in the step (6) in a vacuum furnace for annealing treatment to obtain the QTi3.5/Cu/TiN-Ni-Cu-Re gradient composite coating.
2. The method according to claim 1, wherein in the step (1), ultrasonic cleaning is carried out in an acetone solution for 10-15min, and ultrasonic cleaning is carried out in an absolute ethanol solution for 5-10 min; in the step (2), the surface mechanical grinding treatment time is 20-60 min; in the step (3), the QTi3.5 matrix is ultrasonically cleaned in an acetone solution for 10-15min and in a mixed acid solution for 5-10s, and the mass ratio of the mixed acid cleaning solution is H 2 SO 4 :HNO 3 The ultrapure water is 5:3: 2; in the step (5), the sputtering treatment time is 3-5 min; in the step (6), the sputtering cleaning time is 8-15min, and the reaction is carried outThe co-sputtering time is 40-80 min; in the step (7), the annealing time is 90-150 min.
3. The method as claimed in claim 1, wherein in the step (2), the number of zirconia balls is 180-220, and the diameter of the balls is 4-6 mm; in the step (4), the included angle is 50-75 degrees, and the distance is 60-90 mm.
4. The method as claimed in claim 1, wherein in step (5), the temperature is raised to 100-150 ℃; in the step (7), the annealing temperature is 300-.
5. The method according to claim 1, wherein in the step (2), the vibration frequency of the mechanical grinding treatment is 40-60 Hz; in the step (5), the power of the copper target direct current power supply is 150-; in the step (6), during sputtering cleaning, the RF power of the industrial pure titanium TA1 target is 150-250W, the RF power of the Ni-Cu-Re target is 120-160W, during reactive co-sputtering, the RF power of the industrial pure titanium TA1 target is 180-250W, and the RF power of the Ni-Cu-Re target is 140-180W.
6. The method of claim 1, wherein in step (5), the sputtering chamber vacuum is ≦ 6 x 10 -3 Pa, argon pressure is 3-5 Pa; in the step (6), the argon pressure is 0.5-1.8Pa, and the nitrogen flow is 20-50 sccm; in the step (7), the vacuum degree of the vacuum furnace is less than or equal to 3 multiplied by 10 -2 Pa。
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