A FeCoCuSi-based plug and socket pin material with a multi-layer composite structure and a preparation method thereof

Abstract

The present invention discloses a FeCoCuSi-based plug and socket pin material with a multi-layer composite structure, which is composed of a friction film, a bearing transition layer and a matrix bearing layer. The friction film and the bearing transition layer are mainly made of FeCoCuSi alloy, friction reducer, anti-wear agent and reinforcing agent respectively, and the matrix bearing layer is mainly made of FeCoCuSi alloy. At the same time, a corresponding preparation method thereof is provided. The plug and socket pin material with a multi-layer composite structure prepared by the present invention has fine grains, consistent grain orientation, good purity, high density in each layer material, excellent compressive performance and good compatibility. Each layer has different functions and good synergistic lubrication performance; a large amount of friction reducer and anti-wear agent are distributed in the friction film, and a certain amount of reinforcing agent is added to assist, so that it has good tribological characteristics in a wide temperature range, and excellent tribological performance can be obtained in the range of room temperature to 350 °C, with a small friction coefficient, about 0.19-0.30, and a low wear rate, about 2.72-3.53×10<supgt;‑7 < / supgt;cm<supgt;3< / supgt;·N<supgt;‑1< / supgt>·m<supgt;‑1< / supgt>, and it also has excellent antioxidant performance and good corrosion resistance.

Description

Technical Field

[0001] The present invention belongs to the technical field of antifriction and wear-resistant materials such as pin shafts and bushings. Background Art

[0002] The plug-and-pull pin device commonly used in mechanical structure equipment is mainly composed of a plug-and-pull pin, a connecting seat, a spring, a wire rope and a pull plate, and is used for the positioning and disassembly of mechanical parts. It has the advantages of convenience, safety, quickness and repeated plugging and unplugging, and can maintain a high positioning accuracy during the long-term plugging and unplugging process. For example, the patent with the publication number CN201415318Y and the invention name of a plug-and-pull pin device, and the patent with the publication number CN204935537U and the invention name of a plug-and-pull pin device.

[0003] However, at present, the sliding friction and wear resistance performance of the plug-and-pull pin is poor [Gao Jian, Wu Fudi, etc., Finite element analysis of the seal of the plugging device, Aerospace Materials & Technology, 2013(1), 46-49], resulting in large damage to the sliding surface material during the plugging and unplugging process, thereby affecting its positioning accuracy and running stability, leading to a reduction in its reliable performance and a shortening of its service life. Therefore, it is very important and meaningful to design and develop a new type of plug-and-pull pin with excellent lubrication performance. Summary of the Invention

[0004] The purpose of the present invention is to provide a FeCoCuSi-based plug-and-pull pin material with a multi-layer composite structure, and another object of the present invention is to provide its preparation method.

[0005] A FeCoCuSi-based plug-and-pull pin material with a multi-layer composite structure is composed of a friction film, a bearing transition layer and a matrix bearing layer. The friction film and the bearing transition layer are mainly made of FeCoCuSi alloy, antifriction agent, antiwear agent and reinforcing agent respectively, and the matrix bearing layer is mainly made of FeCoCuSi alloy. [[ID=...]] [[ID=...]]

[0006] The antifriction agent is composed of soft metal, nano NbC and nano CBN, the antiwear agent is composed of tabular crystals, balin stone and qingtian stone, and the reinforcing agent is composed of potassium silicate whiskers, niobium borate crystal flakes and molybdenum sulfate crystal flakes.

[0007] In the friction film, the mass fractions of FeCoCuSi alloy, antifriction agent, antiwear agent and reinforcing agent are 9-14wt.%, 24-45wt.%, 23-41wt.% and 15-27wt.% respectively; in the bearing transition layer, the mass fractions of FeCoCuSi alloy, antifriction agent, antiwear agent and reinforcing agent are 31-47wt.%, 15-25wt.%, 14-20wt.% and 21-39wt.% respectively.

[0008] In the friction film, the anti-friction agent mainly consists of 43-62 wt.% soft metal, 19-34 wt.% nano NbC, and 17-29 wt.% nano CBN; the anti-wear agent mainly consists of 41-56 wt.% plate-like crystals, 24-45 wt.% Balin stone, and 11-21 wt.% Qingtian stone; the reinforcing agent mainly consists of 40-62 wt.% potassium silicate whiskers, 26-47 wt.% niobium borate crystal flakes, and 12-21 wt.% molybdenum sulfate crystal flakes; in the load-bearing transition layer, the anti-friction agent mainly consists of 41-54 wt.% nano CBN, 23-36 wt.% nano NbC, and 19-37 wt.% soft metal, the anti-wear agent mainly consists of 43-52 wt.% plate-like crystals, 25-34 wt.% Balin stone, and 15-27 wt.% Qingtian stone, and the reinforcing agent mainly consists of 27-51 wt.% potassium silicate whiskers, 24-44 wt.% niobium borate crystal flakes, and 18-32 wt.% molybdenum sulfate crystal flakes.

[0009] The soft metal is a soft metal AgZnCuMg alloy, and the soft metal AgZnCuMg alloy is mainly composed of Ag, Zn, Cu, and Mg elements. The mass ratio of Ag, Zn, Cu, and Mg elements of the soft metal in the friction film is (29-45):(21-39):(18-29):(4-9); the mass ratio of Ag, Zn, Cu, and Mg elements of the soft metal in the load-bearing transition layer is (33-43):(25-38):24:5; the FeCoCuSi alloy is mainly composed of Fe, Co, Cu, and Si elements, and the mass ratio of Fe, Co, Cu, and Si elements is (51.7-62.3):21.3:16.5:6; the plate-like crystal is a MoBNbSiO multi-layer plate-like crystal.

[0010] Preparation method of the MoBNbSiO multi-layer plate-like crystal: Grind and mix ammonium molybdate, boron powder, niobium powder, and silicon powder according to a molar ratio of (5-7):(3-4):(2-4):(2-3), and place them in a vacuum atmosphere furnace at a temperature of 525-585 °C with argon as the protective gas for heat preservation for 13.5-16.5 h. Oxygen is introduced during the heat preservation process, and the oxygen introduction amount is 105-129 ml / min to obtain the MoBNbSiO multi-layer plate-like crystal.

[0011] The thickness ratio of the friction film, the load-bearing transition layer, and the matrix load-bearing layer is (8-13):(20-40):(45-72).

[0012] Method for preparing FeCoCuSi-based plug and socket pin material with multi-layer composite structure, the friction film, the load-bearing transition layer and the matrix load-bearing layer are prepared layer by layer. The raw materials of each layer are mixed, hot-pressed and sintered to obtain the friction film sheet, the load-bearing transition layer sheet and the matrix load-bearing layer sheet. After milling, grinding, polishing and lapping them respectively, they are sintered by spark plasma sintering and post-treated to obtain the FeCoCuSi-based plug and socket pin material with multi-layer composite structure.

[0013] Hot-pressing and sintering conditions: pressure 15 - 23 MPa, pressing temperature 125 - 225 °C, heat preservation and pressure holding time 115 - 157 min. Starting from 90 min of heat preservation and pressure holding, deflation is carried out for 4 - 9 s every 25 - 45 s, and the operation is repeated 3 - 7 times; Spark plasma sintering conditions: sintering temperature 973 - 1042 °C, sintering pressure 24 - 29 MPa, heat preservation time 143 - 189 min, heating rate 110 - 125 °C / min, and the protective gas is argon.

[0014] When preparing the friction film, the hot-pressing and sintering conditions: pressure 20 - 23 MPa, pressing temperature 200 - 225 °C, heat preservation and pressure holding time 145 - 157 min. Starting from 90 min of heat preservation and pressure holding, deflation is carried out for 7 - 9 s every 40 - 45 s, and the operation is repeated 5 - 7 times; When preparing the load-bearing transition layer, the hot-pressing and sintering conditions: pressure 18 - 20 MPa, pressing temperature 185 - 210 °C, heat preservation and pressure holding time 135 - 142 min. Starting from 90 min of heat preservation and pressure holding, deflation is carried out for 5 - 7 s every 30 - 35 s, and the operation is repeated 4 - 6 times; When preparing the matrix load-bearing layer, the hot-pressing and sintering conditions: pressure 15 - 19 MPa, pressing temperature 125 - 155 °C, heat preservation and pressure holding time 115 - 130 min. Starting from 90 min of heat preservation and pressure holding, deflation is carried out for 4 - 6 s every 25 - 30 s, and the operation is repeated 3 - 7 times.

[0015] When preparing the method for FeCoCuSi-based plug and socket pin material, the raw material powders of each layer are mixed by a vibrating mixer respectively, the vibration frequency is 64 - 82 Hz, the vibration force is 9940 - 11450 N, and the oscillation time is 145 - 173 min.

[0016] After the friction film sheet, the load-bearing transition layer sheet, and the matrix load-bearing layer sheet are milled, ground, polished, and lapped, the original sheet of the multi-layer structure by spark plasma sintering is obtained. Among them, the rotation speed of the milling machine is 975 - 1053 r / min, and the single-sided milling thickness is 0.3 - 0.6 mm; the rotation speed of the grinding process is 1259 - 1422 r / min, and the grinding thickness is 0.4 - 0.7 μm; after the surface of the sample is polished with sandpaper with a particle size of 1500 - 2500 mesh, wet grinding is carried out with a diamond abrasive with a particle size of 0.02 - 0.05 µm, and sintered and pressed sheets with a diameter of 43 - 52 mm and surface texture structure height parameters Sa of 0.37 - 0.58 µm, Sq of 0.38 - 0.59 µm, Sku of 6.87 - 8.41, and Ssk of 0.16 - 0.39 are obtained. Then, the pressed sheets are loaded into a graphite mold with a diameter of 45 - 55 mm for spark plasma sintering, with a sintering temperature of 973 - 1042 °C, a sintering pressure of 24 - 29 MPa, a heat preservation time of 143 - 189 min, an inert gas of argon, and a heating rate of 110 - 125 °C / min.

[0017] The post-treatment includes turning, grinding, polishing, and electrostatic spraying. The turning speed is 1100 - 1220 r / min, and the turning thickness is 0.75 - 1.35% of the total thickness of the plug and socket sample material. The rotation speed of the grinding process is 1014 - 1235 r / min. The burrs and flash on the periphery are polished and cleaned. The rotation speed of the electrostatic spraying process equipment is 1032 - 1354 r / min, and the temperature is 45 - 50 °C, etc. for post-treatment, and a friction experiment sample of FeCoCuSi-based plug and socket material with a multi-layer composite structure is obtained.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] 1) Through material design and composition formulation, the present invention reduces the content of the friction reducer and anti-wear agent layer by layer, and increases the content of the reinforcing agent and FeCoCuSi alloy component layer by layer, enhancing the bonding performance between the layers of the plug and socket material, overcoming the problem of cracking or damage of each layer under high and low temperature changes, and also providing method guidance and theoretical support for the preparation of coatings and thin films;

[0020] 2) Each layer of the plug and socket material with a multi-layer composite structure prepared by the present invention has fine grains, consistent grain orientation, good purity, high density, excellent compressive performance, good compatibility, different functions of each layer, and good synergistic lubrication performance; a large amount of friction reducer and anti-wear agent are distributed in the friction film, and a certain amount of reinforcing agent is added, making it have good wide-temperature tribological characteristics, enabling it to obtain excellent tribological performance in the range from room temperature to 350 °C, with a small friction coefficient, about 0.19 - 0.30, and a low wear rate, about 2.72 - 3.53×10 -7 cm 3·N -1 ·m -1 and has excellent antioxidant performance and good corrosion resistance;

[0021] 3) The prepared MoBNbSiO multi-layer plate-like crystal has a buffer energy absorption function, which can effectively reduce the impact, vibration and other frictional resistances and the influence of frictional surface damage during the friction process. Distributing it in the friction film and the bearing transition layer can significantly improve the friction reduction and anti-wear performance of the plug and socket pin material, and also provides a new type of solid lubricant for the study of tribological properties;

[0022] 4) The present invention uses FeCoCuSi alloy, friction reducer, anti-wear agent, and strengthener as raw materials, and prepares FeCoCuSi-based plug and socket pin materials with a multi-layer composite structure through processes such as composition design, layered batching, layer-by-layer preparation, and stacking molding. The preparation method is simple in operation and easy to repeat, with good stability, improving work efficiency and being suitable for large-scale batch production. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 is the electron microscope image of the MoBNbSiO powder of the multi-layer plate-like crystal prepared in Example 1;

[0024] Figure 2 is the friction coefficient curve graph of the FeCoCuSi-based plug and socket pin materials prepared in Examples 1, 2, and 3 of the present invention;

[0025] Figure 3 is the bar graph of the wear rate of the FeCoCuSi-based plug and socket pin materials prepared in Examples 1, 2, and 3 of the present invention;

[0026] Figure 4 is the electron microscope morphology image of the bonding state between the bearing transition layer and the matrix bearing layer of the FeCoCuSi-based plug and socket pin material in Example 2;

[0027] Figure 5 is the electron probe image of the friction and wear surface of the FeCoCuSi-based plug and socket pin material in Example 2;

[0028] Figure 6 is the field emission scanning electron microscope image of the friction and wear surface of the FeCoCuSi-based plug and socket pin material in Example 3;

[0029] Figure 7 is the 3D microscopic morphology image of the friction and wear of the FeCoCuSi-based plug and socket pin material in Example 3. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0030] The present invention will be further described below in conjunction with the detailed embodiments and the drawings.

[0031] Example 1

[0032] An FeCoCuSi-based plug and socket pin material with a multi-layer composite structure, which is composed of a friction film, a bearing transition layer and a matrix bearing layer. The friction film and the bearing transition layer are mainly made of FeCoCuSi alloy, friction reducer, anti-wear agent and reinforcing agent respectively, and the matrix bearing layer is mainly made of FeCoCuSi alloy. The total thickness of the friction film, the bearing transition layer and the matrix bearing layer is 10 mm, and the thickness ratio of the three is 8∶20∶45.

[0033] Among them, the friction film is composed of 9 wt.% FeCoCuSi alloy, 24 wt.% friction reducer, 40 wt.% anti-wear agent and 27 wt.% reinforcing agent. The friction reducer is composed of 43 wt.% soft metal AgZnCuMg alloy (mainly composed of Ag, Zn, Cu, Mg, and the mass ratio of the four elements is 29∶21∶18∶4), 29 wt.% nano NbC and 28 wt.% nano CBN. The anti-wear agent is composed of 41 wt.% plate-like crystals (MoBNbSiO multi-layer plate-like crystals), 40 wt.% balin stone and 19 wt.% qingtian stone. The reinforcing agent is composed of 40 wt.% potassium silicate whiskers, 45 wt.% niobium borate crystal flakes and 15 wt.% molybdenum sulfate crystal flakes.

[0034] The bearing transition layer is composed of 31 wt.% FeCoCuSi alloy, 15 wt.% friction reducer, 15 wt.% anti-wear agent and 39 wt.% reinforcing agent. Among them, the friction reducer is composed of 41 wt.% nano CBN, 23 wt.% nano NbC and 36 wt.% soft metal AgZnCuMg alloy (mainly composed of Ag, Zn, Cu, Mg, and the mass ratio of the four elements is 33∶25∶24∶5). The anti-wear agent is composed of 43 wt.% MoBNbSiO multi-layer plate-like crystals, 34 wt.% balin stone and 23 wt.% qingtian stone. The reinforcing agent is composed of 37 wt.% potassium silicate whiskers, 34 wt.% niobium borate crystal flakes and 29 wt.% molybdenum sulfate crystal flakes.

[0035] The bearing layer is made of FeCoCuSi alloy.

[0036] The FeCoCuSi alloy is composed of Fe, Co, Cu, Si, B, Si, Zr and Sc elements, and the mass fraction ratio of the above eight elements is 51.7∶21.3∶16.5∶6∶2.5∶1.0∶0.8∶0.2.

[0037] The MoBNbSiO multi-layer plate-like crystal is composed of molybdenum, boron, niobium, silicon and oxygen elements. The preparation method is as follows: ammonium molybdate, boron powder, niobium powder and silicon powder with a particle size of 37 μm are ground and mixed according to a molar ratio of 5∶3∶2∶2, and placed in a vacuum atmosphere furnace at a temperature of 525 °C with argon as the protective gas for 13.5 h. Argon is used as the protective gas, and oxygen is introduced during the heat preservation process to enhance the reaction. The oxygen flow rate is 105 mL / min to obtain the MoBNbSiO multi-layer plate-like crystal. Its electron microscope image is as shown in Figure 1 shown.

[0038] A method for preparing a FeCoCuSi-based plug and socket material with a multi-layer composite structure includes the following steps:

[0039] 1) Match, calculate and proportion the raw materials required for the friction film, load-bearing transition layer and matrix load-bearing layer, and classify and store the prepared powders for each layer;

[0040] 2) Prepare the friction film, load-bearing transition layer and matrix load-bearing layer layer by layer. The powder of each layer of material is mixed evenly by a vibrating mixer respectively. The vibration frequency is 64 Hz, the vibration force is 9940 N, and the oscillation time is 145 min;

[0041] 3) The powder of each layer of material mixed evenly in step 2) is hot-pressed and sintered to obtain the pressed thin sheet of each layer. When preparing the friction film, the hot-pressing and sintering conditions are: pressure 20 MPa, pressing temperature 200 °C, heat preservation and pressure holding time 145 min. Starting from 90 min of heat preservation and pressure holding, deflation is carried out every 40 s for 7 s, and the operation is repeated 5 times; when preparing the load-bearing transition layer, the hot-pressing and sintering conditions are: pressure 18 MPa, pressing temperature 185 °C, heat preservation and pressure holding time 135 min. Starting from 90 min of heat preservation and pressure holding, deflation is carried out every 30 s for 5 s, and the operation is repeated 4 times; when preparing the matrix load-bearing layer, the hot-pressing and sintering conditions are: pressure 15 MPa, pressing temperature 125 °C, heat preservation and pressure holding time 115 min. Starting from 90 min of heat preservation and pressure holding, deflation is carried out every 25 s for 4 s, and the operation is repeated 3 times;

[0042] 4) The pressed thin sheets of each layer are milled, ground, polished and lapped to obtain the original sintering-ready wafers of each layer. The rotation speed of the milling machine is 975 r / min, and the single-side milling thickness is 0.3 mm; the rotation speed of the grinding process is 1259 r / min, and the grinding thickness is 0.4 μm; after the surface of the sample is polished with sandpaper with a particle size of 1500 mesh, wet grinding is carried out with diamond abrasive with a particle size of 0.02 µm to obtain the original sintering-ready wafers of each layer with a diameter of 43 mm, surface texture height parameters Sa of 0.37 - 0.45 μm, Sq of 0.38 - 0.42 μm, Sku of 6.87 - 7.94 and Ssk of 0.16 - 0.32;

[0043] 5) Transfer the three-layer original green sheets to be sintered into a graphite mold with a diameter of 45 mm. The discharge plasma sintering temperature is 973 °C, the sintering pressure is 24 MPa, the holding time is 143 min, the protective gas is argon, and the heating rate is 110 °C / min to obtain the plug and socket sample material;

[0044] 6) Post-treat the plug and socket sample material, including turning, grinding, polishing, and spraying. The turning speed is 1100 r / min, the turning thickness is 0.93% of the total thickness of the plug and socket sample material, the grinding process speed is 1014 r / min; the polishing machine removes burrs and flash on the periphery, and the electrostatic spraying process equipment speed is 1032 r / min, and the temperature is 45 °C to obtain the FeCoCuSi-based plug and socket material.

[0045] Example 2

[0046] An FeCoCuSi-based plug and socket material with a multi-layer composite structure, which is composed of a friction film, a bearing transition layer, and a matrix bearing layer. The friction film and the bearing transition layer are mainly made of FeCoCuSi alloy, anti-friction agent, anti-wear agent, and reinforcing agent as raw materials, and the matrix bearing layer is mainly made of FeCoCuSi alloy as raw material. The total thickness of the friction film, the bearing transition layer, and the matrix bearing layer is 10 mm, and the thickness ratio of the three is 11∶32∶65.

[0047] The friction film is composed of 12 wt.% FeCoCuSi alloy, 38 wt.% anti-friction agent, 34 wt.% anti-wear agent, and 16 wt.% reinforcing agent. Among them, the anti-friction agent is composed of 54 wt.% soft metal AgZnCuMg alloy (mainly composed of Ag, Zn, Cu, Mg, and the mass ratio of the four elements is 32∶35∶23∶7), 29 wt.% nano NbC, and 17 wt.% nano CBN. The anti-wear agent is composed of 49 wt.% plate-like crystals (MoBNbSiO multi-layer plate-like crystals), 33 wt.% balin stone, and 18 wt.% qingtian stone. The reinforcing agent is composed of 49 wt.% potassium silicate whiskers, 38 wt.% niobium borate crystal flakes, and 13 wt.% molybdenum sulfate crystal flakes.

[0048] The bearing transition layer is composed of 38 wt.% FeCoCuSi alloy, 19 wt.% anti-friction agent, 17 wt.% anti-wear agent, and 26 wt.% reinforcing agent. Among them, the anti-friction agent is composed of 47 wt.% nano CBN, 31 wt.% nano NbC, and 22 wt.% soft metal AgZnCuMg alloy (mainly composed of Ag, Zn, Cu, Mg, and the mass ratio of the four elements is 35∶29∶24∶5). The anti-wear agent is composed of 47 wt.% plate-like crystals (MoBNbSiO multi-layer plate-like crystals), 32 wt.% balin stone, and 21 wt.% qingtian stone. The reinforcing agent is composed of 41 wt.% potassium silicate whiskers, 37 wt.% niobium borate crystal flakes, and 22 wt.% molybdenum sulfate crystal flakes.

[0049] The substrate bearing layer is made of FeCoCuSi alloy.

[0050] The FeCoCuSi alloy is composed of Fe, Co, Cu, Si, B, Si, Zr and Sc elements, and the mass fraction ratio of the eight elements is 60.2∶21.3∶16.5∶6∶2.5∶1.0∶0.8∶0.2.

[0051] The MoBNbSiO multi-layer plate-like crystal is mainly composed of molybdenum, boron, niobium, silicon and oxygen elements. Its preparation method is as follows: ammonium molybdate, boron powder, niobium powder and silicon powder with a particle size of 45 μm are ground and mixed according to a molar ratio of 6∶4∶3∶2, and placed in a vacuum atmosphere furnace at a temperature of 565 °C with argon as the protective gas for heat preservation for 14.8 h. Argon is used as the protective gas, and oxygen is introduced during the heat preservation process to enhance the reaction. The oxygen flow rate is 113 mL / min to obtain the MoBNbSiO multi-layer plate-like crystal.

[0052] A method for preparing a FeCoCuSi-based plug and socket pin material with a multi-layer composite structure includes the following steps:

[0053] 1) Match, calculate and proportion the raw materials required for the friction film, the bearing transition layer and the substrate bearing layer, and classify and store the prepared powders for each layer;

[0054] 2) Prepare the friction film, the bearing transition layer and the substrate bearing layer layer by layer. The powder of each layer of material is respectively mixed evenly by a vibrating mixer. The vibration frequency is 73 Hz, the vibration force is 10952 N, and the oscillation time is 164 min;

[0055] 3) The powders of each layer of material mixed evenly in step 2) are sintered by hot pressing to obtain the pressed thin sheets of each layer. When preparing the friction film, the hot pressing sintering conditions are: pressure 22 MPa, pressing temperature 215 °C, heat preservation and pressure holding time 149 min. Starting from 90 min of heat preservation and pressure holding, air is released for 8 s every 42 s, and the operation is repeated 6 times; when preparing the bearing transition layer, the hot pressing sintering conditions are: pressure 19 MPa, pressing temperature 197 °C, heat preservation and pressure holding time 139 min. Starting from 90 min of heat preservation and pressure holding, air is released for 6 s every 33 s, and the operation is repeated 5 times; when preparing the substrate bearing layer, the hot pressing sintering conditions are: pressure 17 MPa, pressing temperature 145 °C, heat preservation and pressure holding time 125 min. Starting from 90 min of heat preservation and pressure holding, air is released for 5 s every 28 s, and the operation is repeated 5 times;

[0056] 4) Milling, grinding, polishing and lapping the pressed thin sheets of each layer to obtain the original sintering-ready wafers of each layer. The rotational speed of the milling machine is 1000 r / min, and the thickness of the single-side milling is 0.4 mm; the rotational speed of the grinding process is 1322 r / min, and the grinding thickness is 0.6 μm; after polishing the surface of the specimen with sandpaper with a particle size of 2000 mesh, wet grinding is carried out with diamond abrasive with a particle size of 0.04 µm to obtain the original sintering-ready wafers of each layer with a diameter of 47 mm, surface texture height parameters Sa of 0.43 - 0.52 μm, Sq of 0.42 - 0.50 μm, Sku of 6.87 - 7.21 and Ssk of 0.18 - 0.24;

[0057] 5) Transfer the three original sintering-ready wafers into a graphite mold with a diameter of 49 mm. The discharge plasma sintering temperature is 1011 °C, the sintering pressure is 25 MPa, the heat preservation time is 167 min, the protective gas is argon, and the heating rate is 121 °C / min to obtain the plug and socket sample material;

[0058] 6) Post-treat the plug and socket sample material, including turning, grinding, polishing and spraying. The rotational speed of turning is 1193 r / min, and the turning thickness is 0.93% of the total thickness of the plug and socket sample material; the rotational speed of the grinding process is 1133 r / min; the polishing machine removes the burrs and flash around, and the rotational speed of the electrostatic spraying process equipment is 1235 r / min and the temperature is 47 °C to obtain the FeCoCuSi-based plug and socket material.

[0059] The SEM morphology diagram of the bonding state between the load-bearing transition layer and the matrix load-bearing layer of the FeCoCuSi-based plug and socket material prepared in this example is as Figure 4 shown. The electron probe diagram of the friction and wear surface of the FeCoCuSi-based plug and socket material is as Figure 5 shown.

[0060] Example 3

[0061] A FeCoCuSi-based plug and socket material with a multi-layer composite structure, which is composed of a friction film, a load-bearing transition layer and a matrix load-bearing layer. The friction film and the load-bearing transition layer are mainly made of FeCoCuSi alloy, anti-friction agent, anti-wear agent and reinforcing agent as raw materials, and the matrix load-bearing layer is mainly made of FeCoCuSi alloy as raw material. The total thickness of the friction film, the load-bearing transition layer and the matrix load-bearing layer is 10 mm, and the thickness ratio of the three is 13∶40∶72.

[0062] The friction film is composed of 10 wt.% FeCoCuSi alloy, 25 wt.% friction reducer, 38 wt.% anti-wear agent and 27 wt.% reinforcing agent. The friction reducer is composed of 44 wt.% soft metal AgZnCuMg alloy (mainly composed of Ag, Zn, Cu, and Mg elements, and the mass ratio of the four elements is 45∶39∶29∶9), 27 wt.% nano NbC and 29 wt.% nano CBN. The anti-wear agent is composed of 41 wt.% plate-like crystals (MoBNbSiO multi-layer plate-like crystals), 38 wt.% Balin stone and 21 wt.% Qingtian stone. The reinforcing agent is composed of 41 wt.% potassium silicate whiskers, 38 wt.% niobium borate crystal flakes and 21 wt.% molybdenum sulfate crystal flakes.

[0063] The load-bearing transition layer is composed of 33 wt.% FeCoCuSi alloy, 25 wt.% friction reducer, 20 wt.% anti-wear agent and 22 wt.% reinforcing agent. Among them, the friction reducer is composed of 41 wt.% nano CBN, 23 wt.% nano NbC and 36 wt.% soft metal AgZnCuMg alloy (mainly composed of Ag, Zn, Cu, and Mg elements, and the mass ratio of the four elements is 43∶38∶24∶5). The anti-wear agent is composed of 48 wt.% plate-like crystals (MoBNbSiO multi-layer plate-like crystals), 25 wt.% Balin stone and 27 wt.% Qingtian stone. The reinforcing agent is composed of 41 wt.% potassium silicate whiskers, 34 wt.% niobium borate crystal flakes and 25 wt.% molybdenum sulfate crystal flakes.

[0064] The matrix load-bearing layer is made of FeCoCuSi alloy.

[0065] The FeCoCuSi alloy is composed of Fe, Co, Cu, Si, B, Si, Zr and Sc elements, and the mass fraction ratio of the eight elements is 62.3∶21.3∶16.5∶6∶2.5∶1.0∶0.8∶0.2.

[0066] The MoBNbSiO multi-layer plate-like crystal is composed of molybdenum, boron, niobium, silicon and oxygen elements. Its preparation method is as follows: Grind and mix ammonium molybdate, boron powder, niobium powder and silicon powder with a particle size of 49 μm in a molar ratio of 7∶4∶4∶3, and place them in a vacuum atmosphere furnace at a temperature of 585℃ with argon as the protective gas for heat preservation for 16.5 h. Argon is used as the protective gas, and oxygen is introduced during the heat preservation process to enhance the reaction. The oxygen flow rate is 129 mL / min to obtain the MoBNbSiO multi-layer plate-like crystal.

[0067] A method for preparing a FeCoCuSi-based plug and socket pin material with a multi-layer composite structure includes the following steps:

[0068] 1) Match, calculate and proportion the raw materials required for the friction film, load-bearing transition layer and matrix load-bearing layer, and classify and store the prepared powders for each layer;

[0069] 2) Prepare the friction film, load-bearing transition layer, and matrix load-bearing layer layer by layer. The powder of each layer of material is mixed evenly by a vibrating mixer respectively. The vibration frequency is 82 Hz, the vibration force is 11450 N, and the oscillation time is 173 min for each layer;

[0070] 3) Sinter the powder of each layer that has been evenly mixed in step 2) by hot pressing to obtain the pressed thin sheet of each layer. When preparing the friction film, the hot pressing sintering conditions are: pressure 23 MPa, pressing temperature 225 °C, heat preservation and pressure holding time 157 min. Starting from 90 min of heat preservation and pressure holding, deflate for 9 s every 45 s, and repeat the operation 7 times; When preparing the load-bearing transition layer, the hot pressing sintering conditions are: pressure 20 MPa, pressing temperature 210 °C, heat preservation and pressure holding time 142 min. Starting from 90 min of heat preservation and pressure holding, deflate for 7 s every 35 s, and repeat the operation 6 times; When preparing the matrix load-bearing layer, the hot pressing sintering conditions are: pressure 19 MPa, pressing temperature 155 °C, heat preservation and pressure holding time 130 min. Starting from 90 min of heat preservation and pressure holding, deflate for 6 s every 30 s, and repeat the operation 7 times;

[0071] 4) Mill, grind, polish, and launder each layer of the pressed thin sheet to obtain the original sintering-ready matching sheets of each layer. The rotational speed of the milling machine is 1053 r / min, and the single-sided milling thickness is 0.6 mm; The rotational speed of the grinding process is 1422 r / min, and the grinding thickness is 0.7 μm; After polishing the surface of the specimen with sandpaper with a particle size of 2500 mesh, wet grind it with diamond abrasive with a particle size of 0.05 µm to obtain the original sintering-ready matching sheets of each layer with a diameter of 52 mm, surface texture height parameters Sa of 0.49 - 0.58 µm, Sq of 0.48 - 0.59 µm, Sku of 7.72 - 8.41, and Ssk of 0.19 - 0.39;

[0072] 5) Transfer the three layers of original sintering-ready matching sheets into a graphite mold with a diameter of 55 mm. The discharge plasma sintering temperature is 1042 °C, the sintering pressure is 29 MPa, the heat preservation time is 189 min, the protective gas is argon, and the heating rate is 125 °C / min to obtain the plug and socket pin specimen material;

[0073] 6) Post-process the plug and socket pin specimen material, including turning, grinding, polishing, and spraying. The turning speed is 1220 r / min, and the turning thickness is 1.35% of the total thickness of the plug and socket pin specimen material. The rotational speed of the grinding process is 1235 r / min; Use a polishing machine to clean the burrs and flash on the periphery. The rotational speed of the electrostatic spraying process equipment is 1354 r / min, and the temperature is 50 °C to obtain the FeCoCuSi-based plug and socket pin material. The field emission scanning electron microscope image of the friction and wear surface of the obtained FeCoCuSi-based plug and socket pin material is as Figure 6 shown. The 3D microscopic morphology map of the friction and wear of the FeCoCuSi-based plug and socket pin material is asFigure 7 as shown

[0074] Performance Test of Example 4

[0075] Friction and wear tests were carried out on the FeCoCuSi-based plug and socket pin materials prepared in Examples 1, 2, and 3, and the friction coefficient curve graphs formed are as Figure 2 shown, and the wear rate is as Figure 3 shown

[0076] From Figure 2 and 3 it can be seen that the friction coefficients of the FeCoCuSi-based plug and socket pin materials in Examples 1-3 are relatively moderate, and the friction coefficients are approximately 0.30, 0.24, and 0.19 in sequence, and the wear rates are relatively low, and their values are approximately 2.72×10 -7 mm 3 / Nm, 3.11×10 -7 mm 3 / Nm, 3.53×10 -7 mm 3 / Nm. This shows that the FeCoCuSi-based plug and socket pin materials prepared in Examples 1-3 of the present invention have excellent friction reduction and wear resistance performance.

Claims

1. A FeCoCuSi-based plug and socket pin material with a multi-layer composite structure, characterized in that, It is composed of a friction film, a bearing transition layer and a matrix bearing layer. The friction film and the bearing transition layer are mainly made of FeCoCuSi alloy, anti-friction agent, anti-wear agent and reinforcing agent respectively, and the matrix bearing layer is mainly made of FeCoCuSi alloy; The anti-friction agent is composed of soft metal, nano NbC and nano CBN, the anti-wear agent is composed of plate-like crystals, Balin stone and Qingtian stone, and the reinforcing agent is composed of potassium silicate whiskers, niobium borate crystal flakes and molybdenum sulfate crystal flakes; In the friction film, the mass fractions of FeCoCuSi alloy, anti-friction agent, anti-wear agent and reinforcing agent are 9-14wt.%, 24-45wt.%, 23-41wt.% and 15-27wt.% respectively; in the bearing transition layer, the mass fractions of FeCoCuSi alloy, anti-friction agent, anti-wear agent and reinforcing agent are 31-47wt.%, 15-25wt.%, 14-20wt.% and 21-39wt.% respectively; In the friction film, the anti-friction agent is mainly composed of 43-62wt.% soft metal, 19-34wt.% nano NbC and 17-29wt.% nano CBN, the anti-wear agent is mainly composed of 41-56wt.% plate-like crystals, 24-45wt.% Balin stone and 11-21wt.% Qingtian stone, and the reinforcing agent is mainly composed of 40-62wt.% potassium silicate whiskers, 26-47wt.% niobium borate crystal flakes and 12-21wt.% molybdenum sulfate crystal flakes; in the bearing transition layer, the anti-friction agent is mainly composed of 41-54wt.% nano CBN, 23-36wt.% nano NbC and 19-37wt.% soft metal, the anti-wear agent is mainly composed of 43-52wt.% plate-like crystals, 25-34wt.% Balin stone and 15-27wt.% Qingtian stone, and the reinforcing agent is mainly composed of 27-51wt.% potassium silicate whiskers, 24-44wt.% niobium borate crystal flakes and 18-32wt.% molybdenum sulfate crystal flakes; The plate-like crystal is a MoBNbSiO multi-layer plate-like crystal.

2. The FeCoCuSi-based plug and socket pin material with a multi-layer composite structure according to claim 1, characterized in that, The soft metal is a soft metal AgZnCuMg alloy, which is mainly composed of Ag, Zn, Cu and Mg elements. The mass ratio of Ag, Zn, Cu and Mg elements of the soft metal in the friction film is (29-45):(21-39):(18-29):(4-9); the mass ratio of Ag, Zn, Cu and Mg elements of the soft metal in the bearing transition layer is (33-43):(25-38):24:5; FeCoCuSi alloy is mainly composed of Fe, Co, Cu and Si elements, and the mass ratio of Fe, Co, Cu and Si elements is (51.7-62.3):21.3:16.5:

6.

3. The FeCoCuSi-based plug and socket pin material with a multi-layer composite structure according to claim 2, characterized in that, Preparation method of MoBNbSiO multi-layer plate-like crystal: Ammonium molybdate, boron powder, niobium powder and silicon powder are ground and mixed according to a molar ratio of (5-7):(3-4):(2-4):(2-3), and placed in a vacuum atmosphere furnace at a temperature of 525-585 °C with argon as the protective gas for heat preservation for 13.5-16.5 h. Oxygen is introduced during the heat preservation process, and the oxygen introduction amount is 105-129 ml / min to obtain MoBNbSiO multi-layer plate-like crystal.

4. The FeCoCuSi-based plug and socket pin material with a multi-layer composite structure according to claim 3, characterized in that, The thickness ratio of the friction film, the load-bearing transition layer and the matrix load-bearing layer is (8-13):(20-40):(45-72).

5. A method for preparing the FeCoCuSi-based plug and socket pin material with a multi-layer composite structure according to any one of claims 1-4, characterized in that, The friction film, the load-bearing transition layer and the matrix load-bearing layer are prepared layer by layer. The raw materials of each layer are mixed, hot-pressed and sintered to obtain a friction film thin sheet, a load-bearing transition layer thin sheet and a matrix load-bearing layer thin sheet. After milling, grinding, polishing and lapping them respectively, they are sintered by spark plasma sintering and post-treated to obtain an FeCoCuSi-based plug and socket material with a multi-layer composite structure.

6. The method for preparing the FeCoCuSi-based plug and socket pin material with a multi-layer composite structure according to claim 5, characterized in that, Hot-pressing and sintering conditions: pressure 15-23 MPa, pressing temperature 125-225 °C, heat preservation and pressure holding time 115-157 min; Spark plasma sintering conditions: sintering temperature 973-1042 °C, sintering pressure 24-29 MPa, heat preservation time 143-189 min, heating rate 110-125 °C / min, and the protective gas is argon.

7. The method for preparing the FeCoCuSi-based plug and socket pin material with a multi-layer composite structure according to claim 6, characterized in that, When preparing the friction film, the hot-pressing and sintering conditions: pressure 20-23 MPa, pressing temperature 200-225 °C, heat preservation and pressure holding time 145-157 min; When preparing the load-bearing transition layer, the hot-pressing and sintering conditions: pressure 18-20 MPa, pressing temperature 185-210 °C, heat preservation and pressure holding time 135-142 min; When preparing the matrix load-bearing layer, the hot-pressing and sintering conditions: pressure 15-19 MPa, pressing temperature 125-155 °C, heat preservation and pressure holding time 115-130 min.

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