CN109930021B - Copper-based silicon dioxide composite material and preparation method thereof - Google Patents
Copper-based silicon dioxide composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a copper-based silicon dioxide composite material and a preparation method thereof, belonging to the technical field of metal materials and preparation thereof. The composite material comprises the following components in percentage by mass: tin: 0.5-10%, graphite: 10-25%, silica: 2-8%, nano-silica: 0-2% and the balance copper. The preparation steps are as follows: batching, ball milling, mixing, cold press molding, pressure sintering and obtaining the finished product. The tensile strength of the copper-based composite material prepared by the invention is higher than 300MPa, the yield strength is equivalent to that of the commonly used copper-based aluminum oxide composite material, and the wear rate is lower than 1 multiplied by 10‑9cm3·J‑1The heat resistance coefficient is higher than 35000, and the heat resistance and wear resistance are better than those of copper-based aluminum oxide composite materials, so that the wear-resistant part made of the material can meet the requirement of long-term normal work of products or equipment under the condition of higher temperature.
Description
Technical Field
The invention relates to a copper-based silicon dioxide composite material and a preparation method thereof, in particular to an alloy used in a high-temperature and high-friction environment and a preparation method thereof, belonging to the technical field of metal materials and preparation thereof.
Background
The copper-based composite material is used as a brake and a braking device of airplanes, automobiles, ships, engineering machinery and the like due to good wear resistance, heat conductivity and the like, and is widely applied to the high-technology fields of electromechanics, aerospace, microelectronics and the like. The research on copper-based composite materials applied at high temperature is long-standing at home and abroad, and industrialized series products such as copper-based composite oxides, carbides, borides, nitrides and the like are formed.
With the development of equipment towards high speed and heavy load, higher requirements are put forward on the wear resistance and heat resistance of the copper-based friction material. The research result of the copper-based composite material shows that: adopts nano Al2O3Nano ZrO 22Oxygen of equal nanometer levelThe copper-based nano composite material prepared by using the compound as a dispersion strengthening phase utilizes a particle strengthening technology to form hard points which are dispersed and distributed in a soft and tough Cu matrix so as to improve the strength and the wear resistance of the material, can keep the high heat-conducting property of copper, improves the high-temperature softening resistance, achieves the effect of comprehensively improving the electric conduction, the strength and the wear resistance, and has the incomparable advantages compared with other strengthening methods. Therefore, the nano oxide material is applied to the copper-based wear-resistant material, and a new way is provided for improving the tribological performance of the wear-resistant material.
According to the domestic and foreign data, Cu/Al is the most studied2O3A composite material. Nano SiO2(n-SiO2) Because of the special structure and the characteristics of light weight, wear resistance, high temperature resistance, corrosion resistance, small thermal expansion coefficient and the like, the heat conduction and the electric conduction performance of the alloy material are still kept at higher level although being reduced, and the price of the alloy material is only nano Al2O3Half of that. However, since n-SiO2Is easy to agglomerate and is not easy to be uniformly dispersed in a copper matrix, so that the prepared SiO2Reinforcing copper-based composite material performance and Cu/Al2O3Compared with the composite material, the composite material has no advantages, so that the n-SiO is prepared2The use of copper as a reinforcing phase in copper matrices has not been widely investigated.
In recent years, copper-based composite materials are increasingly used in various fields as wear-resistant parts. Therefore, a copper-based silicon dioxide composite material with high strength, high wear resistance and low cost is developed and used in a high-temperature environment, so that the copper-based silicon dioxide composite material is applied to the manufacturing of braking parts for the high-temperature environment in the fields of aerospace, automobiles and the like, and has great significance for improving the product quality, prolonging the service life of equipment and the like.
Disclosure of Invention
The first problem to be solved by the invention is to provide a copper-based silicon dioxide composite material with excellent mechanical property, wear resistance, heat resistance, high conductivity and low density, so that the copper-based silicon dioxide composite material can be used in the fields of aerospace, vehicle traffic, microelectronics and the like.
The second problem to be solved by the invention is to provide a preparation method of the copper-based silicon dioxide composite material with excellent mechanical property, wear resistance, heat resistance, low density and high conductivity.
In order to achieve the purpose, the invention adopts the following technical scheme:
a copper-based silicon dioxide composite material, namely a nano-silicon dioxide reinforced copper-based composite material, comprises the following components in percentage by mass: tin: 0.5-10%, graphite: 10-25%, silica: 2-8%, nano-silica: 0-2% and the balance copper.
Preferably, the copper-based composite material comprises the following components in percentage by mass: tin: 1-5%, graphite: 17-20%, silicon dioxide: 3-6%, nano-silica: 0.3-1.5% and the balance copper.
Wherein the mass percentage of the inevitable impurities is less than or equal to 0.1 percent.
The above component elements play the following roles in the composite material:
graphite: the graphite has the function of improving the lubricating property, particularly the high-temperature lubricating property, of the copper-based composite material, but the graphite is soft, so that the mechanical property of the composite material is reduced by adding excessive graphite.
Tin: on the one hand, tin can accelerate the matrix densification process; on the other hand, tin and graphite have excellent synergistic lubrication effect, the antifriction performance of the copper-graphite composite material can be greatly improved by adding tin, the optimal coordination exists in the synergistic lubrication effect of tin and graphite, and experiments prove that better synergistic lubrication effect can be obtained when the mass ratio of Sn to graphite is in the range of 0.5-30.
Silicon dioxide: the copper-based composite material has the effects of improving the wear resistance, hardness and bonding resistance.
Nano silicon dioxide: n-SiO2The high temperature resistance and the wear resistance of the copper-based composite material can be improved, and simultaneously, dislocation motion and grain boundary slippage can be effectively hindered due to the nanometer effect of the copper-based composite material, so that the copper-based composite material has the effect of remarkably improving the strength of a matrix; on the other hand, n-SiO2With SiO2The coupling effect can improve the density of the composite material.
The preparation method of the silicon dioxide reinforced copper-based composite material mainly comprises the processes of raw material mixing, cold press forming and final pressure sintering, and comprises the following specific steps: the preparation method of the copper-based silicon dioxide composite material comprises the following steps: weighing powder according to a ratio, ball-milling the mixed powder of copper powder and nano silicon dioxide in a planetary high-energy ball mill in advance, then placing the mixed powder and all other raw materials into a small V-shaped mixer to be uniformly mixed, and then pressing the powder into a compact in a steel die; and finally sintering the green compact in a bell jar furnace.
In the invention, electrolytic copper, atomized tin powder, flaky natural graphite, micron-sized silicon dioxide and nano-sized silicon dioxide are used as raw materials. The raw materials used were of the following quality: the average particle size of the electrolytic copper powder is less than or equal to 74 mu m, and the purity is more than or equal to 99.9 wt%; the average particle size of the atomized tin powder is 40-50 mu m, and the purity is more than or equal to 98 wt%; the average granularity of the flaky natural graphite is 140-160 mu m, and the purity is more than or equal to 99 wt%; micron-sized SiO2The average particle size is 40-50 mu m, and the water content is less than or equal to 1 wt%; nano SiO2The average particle diameter is 20 to 40 nm.
Firstly, ball-milling copper powder and nano silicon dioxide in a planetary high-energy ball mill for 2-4 h, and then mixing the copper powder and the nano silicon dioxide together with other raw materials in a V-shaped mixer for 3-5 h; the density of the pressed compact is 4-5 g/cm3(ii) a And when the pressed compact is sintered in a bell jar furnace, the sintering pressure is 1.0-4.0 MPa, the sintering temperature is 800-1000 ℃, the average heating rate is 4-7 ℃/min, a hydrogen reducing protective atmosphere is adopted in the sintering process, the sintering time is 20-40 min, and finally the furnace is cooled to room temperature under the protective atmosphere to prepare the finished product.
The copper-based silicon dioxide composite material has the tensile strength of 300-500 MPa, the yield strength of 200-300 MPa, the elongation of 5-15%, the dynamic friction coefficient of 0.054-0.080, the static friction coefficient of 0.12-0.15 and the wear rate of 0.3-1.0 multiplied by 10-9cm3·J-1A heat resistance coefficient of 35000 to 50000, a relative heat resistance of 1.0 to 1.5, and a density of 5.5 to 8 g/cm3Resistivity of 1.8 to 2.8 x 10-8Omega · m, hardness 50-85 Hv. Compared with the copper-based aluminum oxide composite material, the copper-based silicon dioxide composite material prepared by the invention has equivalent tensile mechanical property, better heat conductivity and wear resistance and simultaneously high tensile mechanical propertyThe cost is lower.
Compared with the prior art, the invention has the advantages that:
(1) the mechanical property, the wear resistance and the heat resistance of the alloy are improved by adding the micron-sized silicon dioxide and the nano-sized silicon dioxide; the addition of tin can improve the wear resistance and accelerate the densification process of the matrix; the graphite particles can perform dispersion strengthening on the copper matrix, and the graphite has a self-lubricating effect and good heat resistance, so that the hardness of the copper matrix is improved. The free hard nano particles can be distributed between friction pairs in the friction process to play a role in a ball effect and reduce the friction factor and the wear rate. When n-SiO2The particles are uniformly distributed in the matrix of the copper-based friction material, so that dislocation movement and grain boundary slippage can be effectively hindered, and the strength and heat resistance of the matrix are improved. The copper-based silicon dioxide composite material designed by the invention has good processing performance, and has better heat resistance and wear resistance compared with the copper-based aluminum oxide composite material.
(2) The invention achieves the purpose of improving the comprehensive performance of the composite material by high-energy ball milling in advance to uniformly disperse the nano silicon dioxide in the copper matrix.
(3) The copper-based silicon dioxide composite material prepared by the invention has lower cost.
Detailed Description
The present invention is described in further detail below with reference to examples.
The preparation method of the copper-based silicon dioxide composite material comprises the following preparation steps: proportioning, high-energy ball milling, mixing, cold press molding, pressure sintering and obtaining the finished product. The specific process steps comprise:
(1) high-energy ball milling: weighing electrolytic copper powder (average particle size is less than or equal to 74 mu m, purity is more than or equal to 99.9 wt%), nano SiO2(the average particle size is 20-40 nm) is placed in a planetary high-energy ball mill for ball milling for 2-4 h in advance.
(2) Mixing raw materials: ball-milled copper-nano SiO2Mixed powder, atomized tin powder (average particle size of 40-50 μm and purity of more than or equal to 98 wt%), flaky natural graphite (average particle size of 140-160 μm and purity of more than or equal to 99 wt%), and micron-sized SiO2(the average particle size is 40-50 mu m, and the water content is less than or equal to 1 wt%) and placing the mixture into a small V-shaped mixer to mix for 3-5 h; the quality of the raw materials used in the examples was the same as above.
(2) Cold-press forming: pressing the powder into a steel die with the diameter of 26mm multiplied by 6.5mm to form the powder with the density of 4-5 g/cm3The compact of (1);
(3) and (3) pressure sintering: sintering the pressed blank in a bell jar furnace under the pressure of 1.0-4.0 MPa, wherein the sintering temperature is 800-1000 ℃, the average heating rate is 4-7 ℃/min, adopting a hydrogen reducing protective atmosphere in the sintering process, the sintering time is 20-40 min, and finally, furnace cooling to room temperature in the protective atmosphere to obtain a finished product.
Example 1
The production process flow method comprises the following steps: burdening-ball milling-mixing-cold press molding-pressure sintering-finished product
The specific process is as follows: proportioning copper and nano SiO according to the components shown in Table 12Ball-milling the mixed powder in a high-energy ball mill for 3 hours, and then mixing the mixed powder with other raw materials in a small V-shaped mixer for 3 hours; in that
Pressing the powder into a steel die with the density of 4-5 g/cm3The compact of (1); sintering the pressed compact in a bell jar furnace under the pressure of 1.0MPa, wherein the sintering temperature is 980 ℃, the average heating rate is 6 ℃/min, a reducing protective atmosphere is adopted in the sintering process, the sintering time is 40min, and finally, furnace cooling is carried out to room temperature under the protective atmosphere to obtain the finished product. The properties of the finished product prepared are shown in table 2.
Example 2
The production process flow method comprises the following steps: burdening-ball milling-mixing-cold press molding-pressure sintering-finished product
The specific process is as follows: proportioning copper and nano SiO according to the components shown in Table 12Ball-milling the mixed powder in a high-energy ball mill for 2 hours, and then mixing the mixed powder with other raw materials in a small V-shaped mixer for 5 hours; in that
In a steel die ofThe resultant density is 4-5 g/cm3The compact of (1); sintering the pressed compact in a bell jar furnace under the pressure of 2.5MPa, wherein the sintering temperature is 900 ℃, the average heating rate is 5 ℃/min, a hydrogen reducing protective atmosphere is adopted in the sintering process, the sintering time is 35min, and finally, furnace cooling is carried out to room temperature under the protective atmosphere to obtain the finished product. The properties of the finished product prepared are shown in table 2.
Example 3
The production process flow method comprises the following steps: burdening-ball milling-mixing-cold press molding-pressure sintering-finished product
The specific process is as follows: proportioning copper and nano SiO according to the components shown in Table 12Ball-milling the mixed powder in a high-energy ball mill for 4 hours, and then mixing the mixed powder with other raw materials in a small V-shaped mixer for 5 hours; in that
Pressing the powder into a steel die with the density of 4-5 g/cm3The compact of (1); sintering the pressed compact in a bell jar furnace under the pressure of 3.5MPa, wherein the sintering temperature is 800 ℃, the average heating rate is 5 ℃/min, a reducing protective atmosphere is adopted in the sintering process, the sintering time is 40min, and finally, furnace cooling is carried out under the protective atmosphere to the room temperature, so as to obtain the finished product. The properties of the finished product prepared are shown in table 2.
Example 4
The production process flow method comprises the following steps: burdening-ball milling-mixing-cold press molding-pressure sintering-finished product
The specific process is as follows: proportioning copper and nano SiO according to the components shown in Table 12Ball-milling the mixed powder in a high-energy ball mill for 3 hours, and then mixing the mixed powder with other raw materials in a small V-shaped mixer for 3 hours; in that
Pressing the powder into a steel die with the density of 4-5 g/cm3The compact of (1); sintering the pressed compact in a bell jar furnace under the pressure of 2.0MPa, wherein the sintering temperature is 850 ℃, the average heating rate is 6 ℃/min, a reducing protective atmosphere is adopted in the sintering process, the sintering time is 30min, and finally, furnace cooling is carried out to room temperature under the protective atmosphere to prepare the finished productAnd (5) preparing the product. The properties of the finished product prepared are shown in table 2.
Example 5
The production process flow method comprises the following steps: burdening-ball milling-mixing-cold press molding-pressure sintering-finished product
The specific process is as follows: proportioning copper and nano SiO according to the components shown in Table 12Ball-milling the mixed powder in a high-energy ball mill for 3 hours, and then mixing the mixed powder with other raw materials in a small V-shaped mixer for 4 hours; in that
Pressing the powder into a steel die with the density of 4-5 g/cm3The compact of (1); sintering the pressed compact in a bell jar furnace under the pressure of 3.0MPa, wherein the sintering temperature is 950 ℃, the average heating rate is 6 ℃/min, a reducing protective atmosphere is adopted in the sintering process, the sintering time is 35min, and finally, furnace cooling is carried out to room temperature under the protective atmosphere to obtain a finished product. The properties of the finished product prepared are shown in table 2.
Example 6
The production process flow method comprises the following steps: burdening-ball milling-mixing-cold press molding-pressure sintering-finished product
The specific process is as follows: proportioning copper and nano SiO according to the components shown in Table 12Ball-milling the mixed powder in a high-energy ball mill for 3 hours, and then mixing the mixed powder with other raw materials in a small V-shaped mixer for 3 hours; in that
Pressing the powder into a steel die with the density of 4-5 g/cm3The compact of (1); sintering the pressed compact in a bell jar furnace under the pressure of 1.0MPa, wherein the sintering temperature is 1000 ℃, the average heating rate is 4 ℃/min, a reducing protective atmosphere is adopted in the sintering process, the sintering time is 25min, and finally, furnace cooling is carried out under the protective atmosphere to the room temperature, so as to obtain the finished product. The properties of the finished product prepared are shown in table 2.
Example 7
The production process flow method comprises the following steps: burdening-ball milling-mixing-cold press molding-pressure sintering-finished product
The specific process is as follows: push-watch1, mixing copper and nano SiO2Ball-milling the mixed powder in a high-energy ball mill for 3 hours, and then mixing the mixed powder with other raw materials in a small V-shaped mixer for 3 hours; in that
Pressing the powder into a steel die with the density of 4-5 g/cm3The compact of (1); sintering the pressed compact in a bell jar furnace under the pressure of 4.0MPa, wherein the sintering temperature is 800 ℃, the average heating rate is 7 ℃/min, a reducing protective atmosphere is adopted in the sintering process, the sintering time is 40min, and finally, furnace cooling is carried out to room temperature under the protective atmosphere to obtain the finished product. The properties of the finished product prepared are shown in table 2.
TABLE 1 compositional composition (wt.%) of a copper-based silica composite
TABLE 2 examples and Properties of conventional copper-based composites
According to the invention, by adding tin, graphite, micron-sized silicon dioxide and nano-sized silicon dioxide, the comprehensive mechanical property, wear resistance and heat resistance of the alloy are finally improved, and meanwhile, the alloy is ensured to have good processing performance; finally, the copper-based composite silicon dioxide material can be obtained by a powder metallurgy method.
As shown in Table 2, the tensile strength of the copper-based composite material prepared by the invention is higher than 300MPa, the yield strength is equivalent to that of the commonly used copper-based composite alumina material, and the wear rate is lower than 1.6 multiplied by 10-9cm3·J-1Heat resistance coefficient higher than 27900 and resistivity lower than 3.2X 10-8cm3·J-1Density lower than 8g cm3The heat resistance and the wear resistance are better than those of the copper-based aluminum oxide composite material, so that the wear-resistant part made of the material can meet the requirement of long-term normal work of products or equipment under the condition of higher temperature.
The present invention includes, but is not limited to, the above embodiments, and any equivalent substitutions or partial modifications made under the spirit and principle of the present invention should be considered within the scope of the present invention.
Claims (8)
1. A copper-based silica composite characterized by: the weight percentage composition is as follows: tin: 1-5%, graphite: 17-20%, micron-sized silicon dioxide: 3-6%, nano-silica: 0.3-1.5% of copper, and the balance of copper; the preparation method of the copper-based silicon dioxide composite material comprises the following steps: weighing powder according to a ratio, ball-milling mixed powder of copper powder and nano silicon dioxide in a planetary high-energy ball mill in advance, then putting the mixed powder and other raw materials into a V-shaped mixer to be uniformly mixed, and then pressing the powder into a blank block in a steel die; and finally sintering the green compact in a bell jar furnace.
2. Copper-based silica composite material according to claim 1, characterized in that: the composite material also comprises impurities, and the mass percent of the impurities is less than or equal to 0.1%.
3. A process for the preparation of a copper-based silica composite material according to claim 1 or 2, comprising the steps of: weighing powder according to a ratio, ball-milling mixed powder of copper powder and nano silicon dioxide in a planetary high-energy ball mill in advance, then putting the mixed powder and other raw materials into a V-shaped mixer to be uniformly mixed, and then pressing the powder into a blank block in a steel die; and finally sintering the green compact in a bell jar furnace.
4. The method for producing a copper-based silica composite material according to claim 3, characterized in that: the raw materials adopted are electrolytic copper, atomized tin powder, scale-like natural graphite, micron-sized silicon dioxide and nano-sized silicon dioxide.
5. The method for producing a copper-based silica composite material according to claim 4, characterized in that: the average particle size of the electrolytic copper powder is less than or equal to 74 mu m, and the purity is more than or equal to 99.9 wt%; the average particle size of the atomized tin powder is 40-50 mu m, and the purity is more than or equal to 98 wt%; the average granularity of the flaky natural graphite is 140-160 mu m, and the purity is more than or equal to 99 wt%; micron-sized SiO2The average particle size is 40-50 mu m, and the water content is less than or equal to 1 wt%; nano SiO2The average particle diameter is 20 to 40 nm.
6. The method for producing a copper-based silica composite material according to claim 3, characterized in that: the ball milling time of the copper powder and the nano silicon dioxide in the planetary high-energy ball mill is 2-4 hours, and the mixing time of the copper powder and the nano silicon dioxide in a V-shaped mixer together with other raw materials is 3-5 hours.
7. The method for producing a copper-based silica composite material according to claim 3, characterized in that: the density of the compact is 4-5 g/cm3。
8. The method for producing a copper-based silica composite material according to claim 3, characterized in that: and when the green compact is sintered in a bell jar furnace, the sintering pressure is 1.0-4.0 MPa, the sintering temperature is 800-1000 ℃, the average temperature rise rate is 4-7 ℃/min, a hydrogen reducing protective atmosphere is adopted in the sintering process, the sintering time is 20-40 min, and finally the furnace is cooled to room temperature under the protective atmosphere.
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