阅读说明：本技术 一种高性能铜基固体自润滑复合材料及其制备方法 (High-performance copper-based solid self-lubricating composite material and preparation method thereof ) 是由 李艳敏 柳学全 李金普 施瑜蕾 姜丽娟 黄霞 赵万林 于 2021-08-16 设计创作，主要内容包括：本发明提供一种高性能铜基固体自润滑复合材料及其制备方法,该复合材料由以下重量百分比的原料制成：5％-30％的固体润滑剂,1％-5％的金属氧化物,余量为铜基体；其中,所述铜基体为铜粉或铜合金粉,所述固体润滑剂为羰基镍包石墨复合粉；所述金属氧化物为纳米态氧化铝或纳米态氧化钇中的至少一种。本发明解决了当前铜基固体自润滑复合材料力学强度差、摩擦系数高、磨损率高的问题,制备得到的复合材料兼具优良的力学性能和摩擦学性能,可用于宽温域、高速、耐腐蚀的工况下,且通过复合材料制得的密封件具有长寿命、长期服役“零泄漏”。(The invention provides a high-performance copper-based solid self-lubricating composite material and a preparation method thereof, wherein the composite material is prepared from the following raw materials in percentage by weight: 5-30% of solid lubricant, 1-5% of metal oxide and the balance of copper matrix; wherein the copper matrix is copper powder or copper alloy powder, and the solid lubricant is nickel carbonyl coated graphite composite powder; the metal oxide is at least one of nano-state aluminum oxide or nano-state yttrium oxide. The invention solves the problems of poor mechanical strength, high friction coefficient and high wear rate of the current copper-based solid self-lubricating composite material, the prepared composite material has excellent mechanical property and tribological property, can be used under the working conditions of wide temperature range, high speed and corrosion resistance, and the sealing element prepared from the composite material has long service life and zero leakage in long-term service.)

1. The high-performance copper-based solid self-lubricating composite material is characterized by being prepared from the following raw materials in percentage by weight: 5-30% of solid lubricant, 1-5% of metal oxide and the balance of copper matrix; wherein the copper matrix is copper powder or copper alloy powder, and the solid lubricant is nickel carbonyl coated graphite composite powder; the metal oxide is at least one of nano-state aluminum oxide or nano-state yttrium oxide.

2. The high-performance copper-based solid self-lubricating composite material as claimed in claim 1, wherein the copper powder is electrolytic copper powder with a particle size of 400-600 mesh; preferably, the copper alloy powder is at least one of tin bronze or manganese brass, and the granularity is 400-600 meshes; preferably, the copper alloy powder is at least one of tin bronze 663 or manganese brass HMn58-2, and the granularity is 400-600 meshes.

3. The high-performance copper-based solid self-lubricating composite material as claimed in claim 1 or 2, wherein the nickel carbonyl-coated graphite composite powder is formed by coating nickel carbonyl on the surface of graphite, the nickel carbonyl accounts for 50-80% of the weight of the nickel carbonyl-coated graphite composite powder, and the particle size of the nickel carbonyl-coated graphite composite powder is 300-500 meshes.

4. The high-performance copper-based solid self-lubricating composite material according to claim 3, wherein the particle size of the nano-alumina is 50-200 nm; preferably, the particle size of the nano yttrium oxide is 50-200 nm.

5. A method for preparing the high-performance copper-based solid self-lubricating composite material as claimed in any one of claims 1 to 4, which comprises the following steps: and sequentially carrying out mixing treatment, compression molding and sintering treatment on the raw materials to obtain the composite material, or sequentially carrying out mixing treatment and pressure sintering integrated molding treatment on the raw materials to obtain the composite material.

6. A preparation method according to claim 5, characterized in that the mixing treatment is to select raw materials meeting the requirements for mixing; preferably, before the mixed material is treated, a binder is added into the raw materials meeting the requirements, wherein the binder is at least one of aviation kerosene, engine oil and alcohol, and the binder accounts for 0.5-2% of the weight of the raw materials meeting the requirements; preferably, the mixing treatment is carried out in a three-dimensional mixer, the rotating speed is 600-1200r/min, and the mixing time is 2-4 h.

7. The production method according to claim 5 or 6, wherein the press forming is cold isostatic pressing; preferably, the pressure of the cold isostatic pressing is 150MPa-260MPa, and the pressure maintaining time is 10min-30 min; preferably, the cold isostatic pressing adopts a rubber mold; alternatively, the first and second electrodes may be,

the compression molding is compression molding; preferably, the pressure for compression molding is 300MPa-600MPa, and the pressure maintaining time is 5min-10 min; preferably, the compression molding uses a steel mold.

8. The production method according to claims 5 to 7, wherein the sintering treatment is low-pressure sintering; preferably, the sintering pressure is 6-20MPa, the sintering temperature is 800-1000 ℃, and the sintering time is 5-15 min; preferably, the sintering is carried out in a low-pressure sintering furnace, and the sintering atmosphere is nitrogen or argon; or, the sintering is carried out in a common hot press, and the sintering is carried out in an atmospheric environment; preferably, the low-pressure sintering adopts a graphite mold.

9. The production method according to claim 5, wherein the pressure sintering integrated molding treatment is vacuum hot-press sintering, and the vacuum hot-press sintering is performed in a vacuum state with a degree of vacuum of not less than 1.33 x 10^-1Pa; or the pressure sintering integrated molding treatment is atmosphere hot-pressing sintering, and the atmosphere hot-pressing sintering is carried out in a hydrogen, argon or nitrogen atmosphere;

preferably, the pressure of the pressure sintering integrated molding is 25MPa-50MPa, the temperature is 700-950 ℃, and the time is 4-10 min; the pressure sintering integrated molding adopts a graphite mold.

10. The application of the high-performance copper-based solid self-lubricating composite material in aerospace high-end equipment according to any one of claims 1 to 4, wherein the high-performance copper-based solid self-lubricating composite material is used as a dynamic seal static ring of a hydraulic motor and a hydraulic pump or a gas sealing bush of a transmission case of an aero-engine, the sealing of a fuel regulator of a missile engine and the sealing of a high-pressure high-speed plunger pump for aerospace.

Technical Field

The invention belongs to the technical field of metal-based solid self-lubricating composite materials, and particularly relates to a high-performance copper-based solid self-lubricating composite material and a preparation method thereof.

Background

In the service environment of high-end equipment such as aerospace and the like, the working conditions of the sealing material are often extremely harsh, such as high and low temperature, high speed, corrosion and the like. If the sealing material fails, not only can the pump body be leaked to pollute other components, but also the function of the whole machine can be failed, and disastrous results can be caused. Since the middle of the last century, accidents caused by the failure of sealing elements are countless and costly. Therefore, the development of aerospace sealing materials integrating high mechanical property, long service life, high and low temperature resistance, corrosion resistance and the like is urgently needed. The research starts from the aim, and develops a metal-based solid self-lubricating composite material for sealing to meet the use requirement under the severe environment.

Solid self-lubricating composite materials are popular in the last century, and can be classified into polymer-based solid self-lubricating composite materials, ceramic-based solid self-lubricating composite materials, metal-based solid self-lubricating composite materials and carbon/graphite composite materials according to the difference of matrix materials. The copper-based solid self-lubricating composite material prepared by taking copper as a matrix and graphite as a solid lubricant has wide application in the aerospace field.

At present, although there are many reports on the preparation of composite materials by using copper as a base material and graphite as a solid lubricant, the preparation is mostly limited to the preparation by processes of simply mixing copper, graphite or other alloy elements, then carrying out re-sintering and re-pressing, forging or hot dipping after sintering, and the like, so that the preparation cost is high, the process period is long, and the obtained composite materials are often high in friction coefficient and wear rate or cannot obtain both the tribological performance and the mechanical strength due to component segregation and material softness, or lead and other toxic elements are used to pollute the environment.

Disclosure of Invention

Aiming at the defects of the prior art, the invention aims to provide a high-performance copper-based solid self-lubricating composite material and a preparation method thereof, which solve the problems of poor mechanical strength, high friction coefficient and high wear rate of the current copper-based solid self-lubricating composite material, and the prepared composite material has excellent mechanical property and tribological property, can be used under the working conditions of wide temperature range, high speed and corrosion resistance, and a sealing element prepared from the composite material has long service life and zero leakage in long-term service; the preparation method has the advantages of easily regulated and controlled raw material components, simple operation, short period and low cost, and can meet increasingly severe environmental protection requirements.

In order to achieve the above object, the first aspect of the present invention provides a high performance copper-based solid self-lubricating composite material, which is prepared from the following raw materials by weight: 5-30% of solid lubricant, 1-5% of metal oxide and the balance of copper matrix; wherein the copper matrix is copper powder or copper alloy powder, and the solid lubricant is nickel carbonyl coated graphite composite powder; the metal oxide is at least one of nano-state aluminum oxide or nano-state yttrium oxide.

In some embodiments, the high-performance copper-based solid self-lubricating composite material is composed of the following raw materials in percentage by weight: 10 to 25 percent of solid lubricant, 1.5 to 3.5 percent of metal oxide and the balance of copper matrix.

In the invention, copper is selected as a base material, compared with metals such as gold, silver, nickel, titanium and the like, the copper is cheaper, and the copper has better performances such as lubrication, heat conduction, electric conduction, corrosion resistance and the like compared with steel; the nickel carbonyl coated graphite composite powder is used as a solid lubricant, graphite can be dissolved in the crystal lattice of nickel in a simple substance form, and simultaneously, the nickel and the copper matrix can form an infinite mutual solution, so that the graphite is uniformly dispersed in the copper matrix, interface pores are greatly reduced, the bonding strength between the solid lubricant and the copper matrix is increased, and the density of the composite material is improved; because graphite is soft, the mechanical property of the composite material is reduced and the wear rate is increased due to the higher adding content, and when the solid lubricant accounts for 5-30% by weight (such as 6%, 10%, 15%, 20%, 25%, 28%) in the raw materials, the composite material has excellent mechanical property and tribological property; preferably 10% to 25%.

According to the invention, at least one of the nano-state aluminum oxide or the nano-state yttrium oxide is added into the copper matrix, and the nano-state aluminum oxide or the nano-state yttrium oxide is not dissolved in the copper matrix and can be uniformly distributed among crystal grains of the copper matrix as a second phase, so that the nano-state aluminum oxide or the nano-state yttrium oxide can play a role in dispersion strengthening when the addition content is low, but can obviously crack the matrix when the addition content is high, thereby reducing the mechanical property of the composite material, and when the weight ratio of the nano-state metal oxide in the raw materials is 1-5% (such as 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%), the composite material has high mechanical strength and low wear rate.

In some embodiments, the copper powder is electrolytic copper powder with a particle size of 400-600 mesh (e.g., 450 mesh, 500 mesh, 550 mesh); preferably, the copper alloy powder is at least one of tin bronze or manganese brass, and the particle size is 400-600 meshes (such as 450 meshes, 500 meshes and 550 meshes); preferably, the copper alloy powder is at least one of tin bronze 663 or manganese brass HMn58-2, and the particle size is 400-600 meshes (such as 450 meshes, 500 meshes and 550 meshes).

In the invention, the copper base material can be electrolytic copper powder, tin bronze powder or manganous brass powder, the electrolytic copper powder has the advantages of small elastic after-effect, good formability, stable technological property and the like, and the mechanical property and the tribological property of the composite material can be improved due to the synergistic effect of alloy elements in the tin bronze powder and the manganous brass powder; the excessive granularity of the electrolytic copper powder, the tin bronze powder or the manganesium powder in the invention can reduce the density of the composite material and deteriorate the hardness and the mechanical property.

In some embodiments, the nickel carbonyl-coated graphite composite powder is graphite surface-coated nickel carbonyl, the nickel carbonyl is 50% to 80% (such as 55%, 60%, 65%, 70%, 75%) of the weight of the nickel carbonyl-coated graphite composite powder, and the particle size of the nickel carbonyl-coated graphite composite powder is 300-500 meshes (such as 350 meshes, 400 meshes, 450 meshes).

In the invention, the nickel carbonyl coated graphite composite powder is prepared by coating nickel carbonyl on the surface of graphite, and the coated particles have the advantages of high nickel purity, uniform thickness and consistent particle size; when the coating amount of the nickel carbonyl is less, on one hand, the effect of enhancing the bonding strength of the solid lubricant and the copper matrix cannot be well played, and on the other hand, the solid lubricant cannot be well uniformly dispersed in the copper matrix; when the coating amount of the nickel carbonyl is too much, on one hand, the content of graphite is reduced, so that the wear resistance of the composite material is reduced, and on the other hand, the cost of the composite material is increased due to the higher price of the nickel; the nickel carbonyl coated graphite composite powder has too small particle size and too many particles, so that the interfacial pores of the composite material are increased, and the strength of the composite material is reduced; the nickel carbonyl coated graphite composite powder has overlarge granularity, obvious fracture can be generated on a matrix, and the mechanical property of the composite material is reduced.

In some embodiments, the nano-alumina has a particle size of 50-200nm (e.g., 60nm, 80nm, 120nm, 150nm, 180 nm); preferably, the particle size of the nano-yttrium oxide is 50-200nm (such as 60nm, 80nm, 120nm, 150nm, 180 nm).

In the invention, the nanometer alumina or nanometer yttrium oxide has too small particle size and is easy to agglomerate, thus not playing the role of dispersion strengthening, and the nanometer alumina or nanometer yttrium oxide has too large particle size and is easy to cause stress concentration and destroy the mechanical property of the composite material.

The invention provides a preparation method of a high-performance copper-based solid self-lubricating composite material, which comprises the following steps: and sequentially carrying out mixing treatment, compression molding and sintering treatment on the raw materials to obtain the composite material, or sequentially carrying out mixing treatment and pressure sintering integrated molding treatment on the raw materials to obtain the composite material.

In some embodiments, the mixing process is to select raw materials meeting the requirements for mixing; preferably, before the mixing treatment, a binder is added to the raw materials meeting the requirement, wherein the binder is at least one of aviation kerosene, engine oil and alcohol, and the binder is 0.5-2% (such as 0.8%, 1.2%, 1.4%, 1.6%, 1.8%) of the raw materials meeting the requirement by weight; preferably, the mixing treatment is carried out in a three-dimensional mixer at a rotation speed of 600-.

In the invention, the raw materials in the range meeting the requirements are selected and mixed by the three-dimensional mixer, so that the particle size distribution of the raw material powder is more concentrated, and the mixing is more uniform; the addition of the binder can ensure that the nickel carbonyl-coated graphite composite powder and the nano metal oxide are not easy to agglomerate and segregate, so that the prepared mixed material can be dispersed more uniformly.

In some embodiments, the press forming is cold isostatic pressing; preferably, the pressure of the cold isostatic pressing is 150MPa-260MPa (such as 170MPa, 190MPa, 210MPa, 230MPa, 250MPa), and the holding time is 10min-30min (such as 15min, 18min, 21min, 24min, 27 min); preferably, the cold isostatic pressing adopts a rubber mold;

in some embodiments, the compression molding is compression molding; preferably, the pressure for compression molding is 300MPa-600MPa (such as 350MPa, 400MPa, 450MPa, 500MPa, 550MPa), and the pressure holding time is 5min-10min (such as 6min, 7min, 8min, 9 min); preferably, the compression molding uses a steel mold. In the invention, the purpose of the compression molding is to process the uniformly mixed powder into a green body with a certain shape and density, so as to be beneficial to subsequent sintering, and further obtain the composite material with higher density.

In some embodiments, the sintering process is low pressure sintering; preferably, the sintering pressure is 6-20MPa (such as 8MPa, 10MPa, 12MPa, 14MPa, 16MPa, 18MPa), the sintering temperature is 800-; preferably, the sintering is carried out in a low-pressure sintering furnace, and the sintering atmosphere is nitrogen or argon; or, the sintering is carried out in a common hot press, and the sintering is carried out in an atmospheric environment; preferably, the low-pressure sintering adopts a graphite mold. In the invention, the green body after press forming can obtain a composite material with high density after low-pressure sintering treatment, if the sintering temperature is too low, the density may not meet the requirement, and if the sintering temperature is too high, the green body may be over-sintered, and uneven structure is easy to occur.

In some embodiments, the pressure sintering integrated forming process is vacuum hot-pressing sintering, and the vacuum hot-pressing sintering is performed in a vacuum state, wherein the vacuum degree is not lower than 1.33 × 10^-1Pa；

In some embodiments, the pressure sintering integrated molding process is an atmospheric hot press sintering performed under a hydrogen, argon, or nitrogen atmosphere;

in some embodiments, the pressure of the pressure sintering integrated molding is 25MPa to 50MPa (such as 30MPa, 35MPa, 40MPa, 45MPa), the temperature is 700 and 950 ℃ (such as 750 ℃, 800 ℃, 850 ℃, 900 ℃) and the time is 4 to 10min (such as 5min, 6min, 7min, 8min, 9 min); the pressure sintering integrated molding adopts a graphite mold.

In the invention, the copper-based solid self-lubricating composite material with excellent mechanical property and tribological property can be prepared by carrying out sintering treatment and pressure sintering integrated forming treatment after compression forming, wherein the preparation method of carrying out sintering treatment after compression forming has lower requirements on equipment but longer production period, and the pressure sintering integrated forming treatment has higher requirements on equipment but short production period.

The third aspect of the invention provides application of a high-performance copper-based solid self-lubricating composite material in aerospace high-end equipment, and the high-performance copper-based solid self-lubricating composite material is used as sealing materials for dynamic sealing static rings of hydraulic motors and hydraulic pumps or gas sealing bushes of transmission casings of aero-engines, sealing of fuel regulators of missile engines, sealing of high-pressure and high-speed plunger pumps for aerospace and the like.

Compared with the prior art, the invention has the following positive effects:

(1) the invention adopts the powder metallurgy process to prepare the high-performance copper-based solid self-lubricating composite material, the raw material components are easy to regulate and control, the operation is simple, the production process parameters are easy to control, the period is short, and the cost is low.

(2) The solid lubricant adopts nickel carbonyl coated graphite composite powder; graphite can be dissolved in the crystal lattice of nickel in a simple substance form, and simultaneously, the nickel and the copper matrix can form an infinite mutual solution, so that the graphite is uniformly dispersed in the copper matrix, thereby greatly reducing the interface pores, increasing the bonding strength between the solid lubricant and the copper matrix and simultaneously improving the density of the composite material.

(3) The high-performance copper-based solid self-lubricating composite material prepared by the invention has high mechanical property, the hardness is more than or equal to 60HB, the crushing strength is more than or equal to 300MPa, and the bending strength is more than or equal to 280 MPa; the tribology performance is excellent, the dry friction coefficient with GCr15 steel is less than or equal to 0.2, and the wear rate is less than or equal to 0.40 wt.%/h (load 100N, rotating speed 200r/min, dry friction); can be used in a wide temperature range of-60 ℃ to 425 ℃; linear thermal expansion coefficient less than or equal to 1.65 × E below 450 deg.C^-0.51/K; corrosion resistance; the linear velocity can be resisted more than or equal to 20 m/s.

(4) The high-performance copper-based solid self-lubricating composite material prepared by the invention can be applied to the field of high-end equipment such as aerospace and the like, dynamic sealing static rings of liquid motors and hydraulic pumps for aerospace prepared by the material achieve zero leakage in 120-hour accelerated life tests, and the sealing surfaces of the static rings have no visual wear in examination after test run.

(5) The high-performance copper-based solid self-lubricating composite material prepared by the invention can be applied to sealing materials such as dynamic sealing static rings, shaft sleeves, bushings, gas seals and the like of high-end equipment such as aerospace, petrochemical industry, ocean navigation and the like.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present invention.

The specific embodiment of the invention provides a high-performance copper-based solid self-lubricating composite material, and the adopted preparation method comprises the following steps:

s1, mixing material: selecting raw materials meeting the requirements, adding 0.5-2% of a binder based on the weight of the raw materials, and mixing in a three-dimensional mixer at the rotation speed of 600-;

s2, press forming: putting the mixed material into a rubber mold, and then carrying out cold isostatic pressing treatment with the pressure of 150MPa-260MPa and the time of 10min-30min to obtain a green body; or putting the mixed material into a steel mold, and then carrying out compression molding treatment under the pressure of 300-600 MPa for 5-10 min to obtain a green body;

s3, sintering treatment: loading the green body into a graphite mold, then carrying out low-pressure sintering in a low-pressure sintering furnace under the atmosphere of nitrogen or argon, wherein the sintering pressure is 6-20MPa, the sintering temperature is 800-1000 ℃, the sintering time is 5-15min, and carrying out pressure relief cooling to obtain the high-performance copper-based solid self-lubricating composite material; or putting the green body into a graphite mold, then sintering at low pressure in an ordinary hot press in the atmospheric environment, wherein the sintering pressure is 6-20MPa, the sintering temperature is 800-1000 ℃, the sintering time is 5-15min, and carrying out pressure relief cooling to obtain the high-performance copper-based solid self-lubricating composite material;

or the preparation method of the high-performance copper-based solid self-lubricating composite material comprises the following steps:

s1, mixing material: selecting raw materials meeting the requirements, adding 0.5-2% of a binder based on the weight of the raw materials, and mixing in a three-dimensional mixer at the rotation speed of 600-;

s2, pressure sintering integrated molding treatment: loading the mixture into graphite mould, hot-pressing and sintering under vacuum condition with vacuum degree not less than 1.33 × 10^-1Pa, the pressure is 25MPa-50MPa, the temperature is 700-950 ℃, the time is 4-10min, and the high-performance copper-based solid self-lubricating composite material is obtained after pressure relief and cooling; or the mixed material is put into a graphite die, then hot-pressed and sintered under the atmosphere of hydrogen, argon or nitrogen, the pressure is 25MPa-50MPa, the temperature is 700-950 ℃, the time is 4-10min, and the high-performance copper-based solid self-lubricating composite material is obtained after pressure relief and cooling.

The raw materials used in the following examples are commercially available, and the instruments, equipment and the like are commercially available.

Example 1

A high-performance copper-based solid self-lubricating composite material adopts a preparation method comprising the following steps:

s1, mixing material: selecting 100g of nickel carbonyl-coated graphite composite powder with the granularity of 300 meshes and the nickel carbonyl content of 60.5 wt% and nano Al with the granularity of 200nm₂O₃15g of powder and 885g of electrolytic copper powder with the granularity of 400 meshes, adding 8g of binder (aviation kerosene) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 650r/min for 3.5h to obtain a mixed material;

s2, press forming: putting the mixed materials into a steel mold, and then carrying out compression molding treatment under the pressure of 400MPa for 8min to obtain a green body;

s3, sintering treatment: and (2) putting the green body into a graphite mold, then carrying out low-pressure sintering in a low-pressure sintering furnace under the argon atmosphere, wherein the sintering pressure is 10MPa, the sintering temperature is 940 ℃, the sintering time is 13min, and carrying out pressure relief cooling to obtain the high-performance copper-based solid self-lubricating composite material.

Example 2

A high-performance copper-based solid self-lubricating composite material adopts a preparation method comprising the following steps:

s1, mixing material: selecting 100g of nickel carbonyl-coated graphite composite powder with the granularity of 300 meshes and the nickel carbonyl content of 60.5 wt% and selecting nano Y with the granularity of 200nm₂O₃15g of powder and 885g of tin bronze 663 powder with the granularity of 400 meshes, adding 12g of binder (engine oil) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 650r/min for 3.5h to obtain a mixed material;

s2, press forming: putting the mixed materials into a steel mold, and then carrying out compression molding treatment under the pressure of 400MPa for 8min to obtain a green body;

s3, sintering treatment: and (2) putting the green body into a graphite mold, then carrying out low-pressure sintering in an ordinary hot press in an atmospheric environment, wherein the sintering pressure is 18MPa, the sintering temperature is 910 ℃, the sintering time is 7min, and carrying out pressure relief cooling to obtain the high-performance copper-based solid self-lubricating composite material.

Example 3

A high-performance copper-based solid self-lubricating composite material adopts a preparation method comprising the following steps:

s1, mixing material: selecting 100g of nickel carbonyl-coated graphite composite powder with the granularity of 300 meshes and the nickel carbonyl content of 60.5 wt% and selecting nano Y with the granularity of 200nm₂O₃15g of powder and 885g of manganese brass HMn58-2 powder with the granularity of 400 meshes, adding 16g of adhesive (alcohol) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 650r/min for 3.5h to obtain a mixed material;

s2, filling the mixed materials into a rubber mold, and then carrying out cold isostatic pressing forming treatment under the pressure of 250MPa for 24min to obtain a green body;

s3, sintering treatment: and (3) putting the green body into a graphite mold, then carrying out low-pressure sintering in an ordinary hot press in an atmospheric environment, wherein the sintering pressure is 16MPa, the sintering temperature is 970 ℃, the sintering time is 9min, and carrying out pressure relief cooling to obtain the high-performance copper-based solid self-lubricating composite material.

Example 4

A high-performance copper-based solid self-lubricating composite material adopts a preparation method comprising the following steps:

s1, mixing material: selecting 300g of nickel carbonyl coated graphite composite powder with the granularity of 400 meshes and the nickel carbonyl content of 80.0 wt% and selecting nano Al with the granularity of 100nm₂O₃35g of powder and 665g of electrolytic copper powder with the granularity of 400 meshes, adding 12g of binder (aviation kerosene) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 1000r/min for 3.5h to obtain a mixed material;

s2, pressure sintering integrated molding treatment: putting the mixed material into a graphite mould, and then carrying out hot-pressing sintering in a vacuum state, wherein the vacuum degree is 1.33 multiplied by 10^-1Pa, the pressure is 30MPa, the temperature is 850 ℃, the time is 8min, and the high-performance copper-based solid self-lubricating composite material is obtained after pressure relief and cooling.

Example 5

A high-performance copper-based solid self-lubricating composite material adopts a preparation method comprising the following steps:

s1, mixing material: selecting 300g of nickel carbonyl-coated graphite composite powder with the granularity of 400 meshes and the nickel carbonyl content of 80.0 wt% and selecting nano Al with the granularity of 50nm₂O₃35g of powder and 665g of electrolytic copper powder with the granularity of 600 meshes, adding 12g of binder (aviation kerosene) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 1000r/min for 3.8h to obtain a mixed material;

s2, pressure sintering integrated molding treatment: and (2) loading the mixed material into a graphite die, then carrying out hot-pressing sintering under the argon atmosphere, carrying out pressure intensity of 40MPa, temperature of 850 ℃ and time of 7min, and carrying out pressure relief cooling to obtain the high-performance copper-based solid self-lubricating composite material.

Comparative example 1

Comparative example 1 the same as example 1 except that the mixing process of S1 was different from example 1, comparative example 1:

s1, mixing material: selecting 100g of nickel carbonyl-coated graphite composite powder with the granularity of 300 meshes and the content of 60.5 wt% of nickel carbonyl and 885g of electrolytic copper powder with the granularity of 400 meshes, adding 8g of binder (aviation kerosene) to prevent segregation, mixing in a three-dimensional mixer at the rotating speed of 650r/min for 3.5h to obtain a mixed material.

Comparative example 2

Comparative example 2 the same as example 1 except that the mixing process of S1 was different from that of example 1, comparative example 2:

s1, mixing material: selecting 100g of graphite powder with the granularity of 300 meshes and 200nm of nano Al₂O₃15g of powder and 885g of electrolytic copper powder with the granularity of 400 meshes, adding 8g of binder (aviation kerosene) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 650r/min for 3.5h to obtain a mixed material.

Comparative example 3

Comparative example 3 the same as example 1 except that the mixing process of S1 was different from that of example 1, comparative example 3:

s1, mixing material: 39.5g of graphite powder with the granularity of 300 meshes, 60.5g of nickel powder with the granularity of 300 meshes and 200nm of nano Al are selected₂O₃15g of powder and 885g of electrolytic copper powder with the granularity of 400 meshes, adding 8g of binder (aviation kerosene) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 650r/min for 3.5h to obtain a mixed material.

Comparative example 4

Comparative example 4 the same as example 4 except that the mixing treatment of S1 was different from example 4, comparative example 4:

s1: selecting 400g of nickel carbonyl coated graphite composite powder with the granularity of 400 meshes and the nickel carbonyl content of 80.0 wt% and selecting nano Al with the granularity of 100nm₂O₃35g of powder and 565g of electrolytic copper powder with the granularity of 400 meshes, adding 12g of binder (aviation kerosene) to prevent segregation, and mixing in a three-dimensional mixer at the rotating speed of 1000r/min for 3.5h to obtain a mixed material.

Performance detection

The high-performance copper-based solid self-lubricating composite material prepared in the application through the examples 1-5 and the composite material prepared in the comparative examples 1-4 are prepared into a test sample according to corresponding standards and then tested. Wherein the bending resistance test (according to GB/T232-, the results are shown in Table 1.

TABLE 1 results of Performance test of examples 1-5 and comparative examples 1-4

The above description is only exemplary of the invention and should not be taken as limiting the invention, as any modification, equivalent replacement, or improvement made within the spirit and principle of the invention is intended to be covered by the appended claims.