CN111101027B - High-strength high-conductivity high-heat-resistance aluminum-based composite material for splicing fitting and preparation method thereof - Google Patents
High-strength high-conductivity high-heat-resistance aluminum-based composite material for splicing fitting and preparation method thereof Download PDFInfo
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Abstract
The invention provides a high-strength high-conductivity high-heat-resistance aluminum-based composite material for splicing fittings and a preparation method thereof. The graphene has a unique two-dimensional wrinkled surface, copper nano particles are grown on the surface of the graphene to form graphene @ copper, the wettability of the graphene and an aluminum melt is improved, the graphene and the aluminum melt are used as particles for refining grains of non-uniform nucleation, and the graphene has good chemical stability and Al3The Zr phase promotes the thermal stability of the aluminum matrix composite material. The invention solves the problem of limiting the strength and heat resistance in the application process of the 1-series alloy splicing fitting, and the aluminum-based composite material produced by the casting method keeps the electric conductivity higher than 61% IACS, improves the strength by more than 30%, and improves the heat resistance by more than 20-40 ℃.
Description
Technical Field
The invention relates to a nanophase reinforced aluminum-based composite material, in particular to a high-strength high-conductivity high-heat-resistance aluminum-based composite material for splicing fittings and a preparation method thereof.
Background
With the improvement of voltage grade and the application of various novel wires, the abnormal temperature rise of the tension splicing fitting becomes a great potential safety hazard influencing the operation of a line. According to statistics, the temperature of the strain clamp of 16 lines in the Beijing area in 2008 is between 43 and 150 ℃ and is higher than the temperature of an adjacent wire by 19 to 126 ℃, wherein 3 percent of the temperature exceeds 120 ℃ and reaches 150 ℃ at most, the temperature greatly exceeds the regulation that the operating temperature of a splicing fitting and the strain clamp is not higher than the temperature of the adjacent wire by 10 ℃ in the overhead power transmission line operating regulation (DLT/741 plus 2010), accidents caused by abnormal temperature rise, failure and falling of the strain splicing fitting of the wire are rare in China, materials for high-performance strain splicing fittings are researched, and the strain splicing fittings are inevitably popularized and applied in a power transmission line. The insufficient crimping grip and the loosening of the crimping zone after long-term operation cause the increase of the connection resistance, which is the main reason of abnormal temperature rise. At present, a tension splicing fitting drainage component is usually manufactured by adopting an electrical pure aluminum section, and a pressure connection area is difficult to avoid loosening too early in the operation of a large-specification line, so that temperature rise is caused. And because of poor heat-resistant stability, the conductivity and mechanical property of the drainage component are obviously reduced along with the increase of the temperature rise amplitude, and the creep is relaxed. The process is vicious and circulated until abnormal temperature rise, and finally the product is invalid and falls off, so that accidents are caused. For high-voltage grade lines, especially extra-high voltage lines, extra-high voltage lines and the like, large-area power failure can be caused, the consequences are serious, and urgent solution is needed. The research on the high-performance hardware fitting material is used for replacing pure aluminum materials in the tension-resistant splicing hardware fitting, so that the material for the drainage component of the tension-resistant splicing hardware fitting has high strength, high conductivity, high thermal stability and high heat dissipation performance, the conduction performance and the anti-relaxation performance of the tension-resistant splicing hardware fitting are improved, the method is an effective way and a key method for solving abnormal temperature rise of a wire splicing part, ensuring long-term stability of crimping grip of a wire and improving the safety and reliability of circuit operation, and has important application value for improving the safety stability of a power transmission and transformation circuit and reducing operation and maintenance cost.
The first preparation in 2004 by England scientists was sp from carbon atoms2Graphene, a novel two-dimensional atomic crystal formed by hybridized and connected monoatomic layers, has the thickness of only 0.3354nm, and is the thinnest material found in the world at present. Graphene has a special monoatomic layer structure and extremely excellent physical properties: the carbon nanotube has the characteristics of 1100GPa of Young modulus and 125GPa of fracture strength, about 5000J/(m.K.s) of thermal conductivity, low thermal expansion coefficient, minimum quantum conductivity under the limit of zero carrier concentration and the like. The graphene with low density and excellent mechanical and thermophysical properties is added into the aluminum alloy as a reinforcing phase, so that the composite material with light weight, high strength, high electric conductivity, high heat conductivity and high thermal stability can be obtained.
At present, few reports about graphene reinforced metal matrix composite materials exist, and the preparation of the materials is in a preliminary exploration stage. For graphene-reinforced metal matrix composites, prior patent 1 (publication No. 104032154 a; 103938011a) employs spark plasma sintering to prepare graphene/metal matrix composite materials. Publication No. 102329976a, "preparation method of graphene-reinforced metal matrix composite", in which graphene oxide is dispersed on the surface of a sheet metal, and then reduced to obtain graphene/metal composite powder, and densification treatment is performed by using a powder metallurgy process to prepare the graphene-reinforced metal matrix composite. Publication No. CN110331316 discloses a high-strength heat-resistant aluminum-based composite conductor material and a preparation method thereof, wherein graphene and aluminum powder are subjected to ball milling and powder mixing, amorphous alumina is obtained on the surface of the graphene, and the composite material is prepared by a powder metallurgy sintering molding method. The publication No. CN105385871A is that nano carbon with the surface coated with metal ion precursor is dispersed into aluminum powder, mixed powder is obtained by heat treatment and sintering, and the heat-resistant aluminum-based composite material is produced by adopting the conventional powder metallurgy process. The publication No. CN108396168A is used for preparing the composite material with the density of 98.5% by mixing graphene and aluminum powder, canning and carrying out semi-solid extrusion. At present, the preparation method of the graphene aluminum-based composite material mainly adopts powder metallurgy, and methods such as sheath extrusion and semi-solid extrusion are also adopted, so that the mold cost is high, the production rate is low, and batch and continuous industrial production is difficult. CN110295298A adopts a hydrothermal method to synthesize alumina @ graphene, the chemical reaction process is complex, the size and the particle size of alumina particles are complex to control, impurities are easily brought into molten aluminum to reduce the conductivity, and the method is not suitable for preparing 1-series conductor materials.
Disclosure of Invention
The invention aims to solve the problems of low strength and insufficient heat resistance of a 1-series alloy for splicing fittings, provides a high-strength high-conductivity high-heat-resistance aluminum-based composite material for splicing fittings and a preparation method thereof, and aims to improve the strength and greatly reduce the application bottleneck problem of conductivity by the traditional alloying technology.
The invention is realized by the following technical scheme:
the invention provides a high-strength high-conductivity high-heat-resistance aluminum-based composite material for splicing fittings, which comprises the following alloy components, by mass, 0.01-0.09% of reduced graphene oxide, 0.05-0.2% of Zr, 0.05-0.2% of Er, 0.008-0.010% of Ti, less than or equal to 0.07% of Fe, less than or equal to 0.05% of Si, and the balance of Al.
In the above high-strength, high-conductivity and high-heat-resistance aluminum-based composite material, preferably, the mass percentage of each of the other elements is not more than 0.01%, and the other elements are elements except reduced graphene oxide, Zr, Er, Ti, Fe, Si and Al in the base composite material. The invention also provides a splicing fitting which is prepared from the high-strength high-conductivity high-heat-resistance aluminum-based composite material for the splicing fitting.
The invention also provides a preparation method of the aluminum matrix composite material, which comprises the following steps:
(1) charging an aluminum ingot into a furnace, and after the aluminum ingot is completely melted, preserving heat for 20-30min at the temperature of 710-;
(2) heating the aluminum melt to 740 ℃ and 760 ℃, adding Al-Er and Al-Zr intermediate alloy, and keeping the temperature of the melt for 10-30 min;
(3) blowing reduced graphene oxide @ copper powder into the aluminum melt by adopting argon, and stirring while blowing until mixed powder is blown in;
(4) blowing argon into a 4AB type refining agent, wherein the adding mass of the refining agent is 1.0-1.2% of the mass of the aluminum melt;
(5) keeping the temperature of the melt static for 8-10min, carrying out slagging-off treatment, discharging, and casting a cast ingot bar;
(6) cutting the head and the tail of the cast ingot, turning surface oxide skin, and then performing extrusion deformation;
(7) and carrying out solid solution aging treatment on the extrusion piece to obtain the high-strength high-conductivity high-heat-resistance aluminum-based composite material.
Preferably, the raw material for preparing the reduced graphene oxide @ copper in the step (3) comprises 1-10 layers of graphene oxide with the sheet diameter of 1-25 microns.
Preferably, the preparation method of the reduced graphene oxide @ copper in the step (3) is as follows: preparing a KH-550 silane coupling agent solution (more preferably, the volume ratio of alcohol to water is 1-10:12-1, the content of KH-550 in the solution is 0.1 vol.% to 0.9 vol.%, and the solution is still dissolved for 4-8 h); adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.1-1g/L, adding nano copper powder for ultrasonic treatment for 30-60min, wherein the particle size of the nano copper powder is 5-30 nm, carrying out hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and obtaining reduced graphene oxide @ copper composite powder after sintering at the temperature of 900-1200 ℃ for 1-5 hours.
Preferably, in the reduced graphene oxide @ copper composite powder, the mass fraction of copper is 1.0-5.0%.
Preferably, the step (6) comprises an extrusion heating operation, wherein the extrusion heating temperature is 300-400 ℃, the heat preservation time is 3-5 hours, and the extrusion ratio is 20-30: 1, extrusion rate 1.0-5.0 mm/min.
Preferably, the solid solution temperature in the step (7) is 560-; the aging temperature is 200 ℃ and 400 ℃, and the heat preservation time is 12-72 hours.
In aluminiumZr and Er are added into the melt, and the two elements can react with Al to generate Al3(Er, Zr) phase, Al3The (Er, Zr) phase presents a nano phase in dispersion distribution, so that the slippage and climbing of dislocation are prevented, the grain boundary and subboundary can be pinned, and the process that the dislocation is rearranged into the subboundary and then developed into a large-angle grain boundary during heating is prevented, so that the nucleation and growth of recrystallization are delayed, the recrystallization temperature of the aluminum alloy matrix is improved, and the heat resistance is improved. However, the addition amounts of Er and Zr and the addition process need to be strictly controlled, and the conductivity is greatly reduced when the addition amount reaches a certain amount, so that the process and the addition amount are obtained through a large number of experiments.
The beneficial effects of the invention include:
(1) the invention adopts common aluminum alloy smelting and casting equipment for production, and uses the traditional inert gas purification equipment to blow the reduced graphene oxide @ copper powder into the aluminum melt for producing large-size components by semi-continuous casting or continuous casting and rolling, so that the structure is uniform, the material is compact, the process is simple, the production efficiency is high, the defects of small size, high mold cost and low material density of the powder metallurgy technology are avoided, and the method is suitable for industrial large-scale production.
(2) According to the invention, the redox graphene @ copper is added into the aluminum melt, so that the interface wettability of the graphene and the aluminum alloy matrix can be improved by the nano-copper, the interface bonding energy between the aluminum alloy and the graphene sheet is further improved, the graphene is uniformly dispersed into the aluminum melt, the reinforcing effect of the graphene is fully exerted, and the aluminum-based composite material with good interface bonding is obtained. In addition, copper is added in the reduction process of the graphene oxide, so that the reduced graphene oxide is prevented from agglomerating in the reduction process, and the agglomeration of the reduced graphene oxide is also obviously reduced after the melt is blown in.
(3) The chemical property of the graphene is kept stable at high temperature, the alloy provided by the invention has good heat resistance, the electric conductivity of the aluminum-based composite material produced by the casting method is kept higher than 61% IACS, the strength is improved by more than 30%, and the heat resistance is improved by more than 20-40 ℃.
Detailed Description
The technical solutions of the present invention will be described in detail below in order to clearly understand the technical features, objects, and advantages of the present invention, but the present invention is not limited to the practical scope of the present invention.
Example 1
Alloy components: by taking the mass of the alloy as 100%, the reduced graphene oxide is 0.09%, the Zr is 0.2%, the Er is 0.1%, the Ti is 0.001%, the Fe is 0.065%, the Si is less than or equal to 0.043, the rest elements are less than or equal to 0.01% each, and the balance is Al.
The preparation process and the proportion of the reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the volume ratio of alcohol to water is 10:1, the content of KH-550 in the solution is 0.9 vol.%, and standing for dissolving for 4 h; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.1g/L, adding nano copper powder for ultrasonic treatment for 60min, enabling the particle size of the nano copper powder to be 5nm, carrying out hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and carrying out sintering at 1200 ℃ for 5 hours to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 750 ℃, and Al-Er and Al-Zr intermediate alloy is added. And blowing the reduced graphene oxide @ copper powder into the aluminum melt by using argon, and fully stirring the melt by using a stirring tool until the reduced graphene oxide @ copper powder is blown. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 400 ℃, the heat preservation is carried out for 3 hours, and the extrusion ratio is 20: 1, extrusion rate 4.0 mm/min; finally, carrying out solid solution treatment and aging treatment, wherein the solid solution temperature is 600 ℃, and the heat preservation time is 5 hours; the aging temperature is 400 ℃, and the heat preservation time is 48h, so that the aluminum matrix composite material is obtained.
Example 2
Alloy components: by taking the mass of the alloy as 100%, 0.01% of reduced graphene oxide, 0.2% of Zr, 0.2% of Er, 0.008% of Ti, 0.070% of Fe, 0.045% of Si, less than or equal to 0.01% of each of the other elements and the balance of Al.
The preparation process and the proportion of the pre-synthesized reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the volume ratio of alcohol to water is 1:12, the content of KH-550 in the solution is 0.1 vol.%, and standing for dissolving for 4 h; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.5g/L, adding nano copper powder for ultrasonic treatment for 30min, wherein the particle size of the nano copper powder is 30nm, performing hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and sintering at 1200 ℃ for 1 hour to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.78 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 760 ℃, and Al-Er and Al-Zr intermediate alloy is added. And blowing the reduced graphene oxide @ copper powder into the aluminum melt by using argon, and fully stirring the melt by using a stirring tool until the reduced graphene oxide @ copper powder is blown. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 350 ℃, the temperature is kept for 3 hours, and the extrusion ratio is 25: 1, extrusion rate 3.0 mm/min; finally, carrying out solid solution treatment and aging treatment, wherein the solid solution temperature is 580 ℃, and the heat preservation time is 4 hours; the aging temperature is 350 ℃, and the heat preservation time is 24h, so that the aluminum matrix composite material is obtained.
Example 3
Alloy components: by taking the mass of the alloy as 100%, the reduced graphene oxide is 0.05%, the Zr is 0.1%, the Er is 0.1%, the Ti is 0.009%, the Fe is 0.068%, the Si is 0.043%, the rest elements are less than or equal to 0.01% each, and the balance is Al.
The preparation process and the proportion of the pre-synthesized reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the volume ratio of alcohol to water is 7: 5, KH-550 is contained in the solution in an amount of 0.5 vol.%, and is statically dissolved for 6 hours; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.5g/L, adding nano copper powder for ultrasonic treatment for 40min, wherein the particle size of the nano copper powder is 20nm, performing hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and performing sintering at 1000 ℃ for 3 hours to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 740 ℃, and Al-Er and Al-Zr intermediate alloy is added. And blowing the reduced graphene oxide @ copper powder into the aluminum melt by using argon, and fully stirring the melt by using a stirring tool until the reduced graphene oxide @ copper powder is blown. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 350 ℃, the temperature is kept for 4 hours, and the extrusion ratio is 22: 1, extrusion rate is 3.0mm/min, and finally solid solution treatment and aging treatment are carried out, wherein the solid solution temperature is 570 ℃, and the heat preservation time is 4 hours; the aging temperature is 380 ℃, and the heat preservation time is 72h, so as to obtain the aluminum matrix composite material.
Example 4
Alloy components: by taking the mass of the alloy as 100%, the reduced graphene oxide is 0.03%, the Zr is 0.15%, the Er is 0.15%, the Ti is 0.0085%, the Fe is 0.069%, the Si is 0.041%, the rest elements are less than or equal to 0.01% each, and the balance is Al.
The preparation process and the proportion of the reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the volume ratio of alcohol to water is 3: 12, KH-550 is contained in the solution in an amount of 0.9 vol.%, and is statically dissolved for 4 hours; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.7g/L, adding nano copper powder for ultrasonic treatment for 50min, wherein the particle size of the nano copper powder is 30nm, carrying out hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and carrying out sintering at 1100 ℃ for 3 hours to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 750 ℃, and Al-Er and Al-Zr intermediate alloy is added. And blowing the reduced graphene oxide @ copper powder into the aluminum melt by using argon, and fully stirring the melt by using a stirring tool until the reduced graphene oxide @ copper powder is blown. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 400 ℃, the heat preservation is carried out for 3 hours, and the extrusion ratio is 20: 1, extruding at a speed of 4.0mm/min, and finally performing solid solution treatment and aging treatment at a solid solution temperature of 600 ℃ for 5 hours; the aging temperature is 400 ℃, and the heat preservation time is 48h, so that the aluminum matrix composite material is obtained.
Example 5
Alloy components: by taking the mass of the alloy as 100%, the reduced graphene oxide is 0.07%, the Zr is 0.08%, the Er is 0.08%, the Ti is 0.009%, the Fe is less than or equal to 0.07%, the Si is less than or equal to 0.05%, the rest elements are less than or equal to 0.01% each, and the balance is Al.
The preparation process and the proportion of the reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the volume ratio of alcohol to water is 10: the content of KH-550 in the solution is 0.3 vol.%, and the solution is statically dissolved for 8 h; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.2g/L, adding nano copper powder for ultrasonic treatment for 30min, wherein the particle size of the nano copper powder is 25nm, carrying out hydrogen reduction sintering on the graphene oxide after vacuum freeze drying treatment of the solution, and carrying out sintering at 900 ℃ for 4 hours to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 750 ℃, and Al-Er and Al-Zr intermediate alloy is added. And blowing the reduced graphene oxide @ copper powder into the aluminum melt by using argon, and fully stirring the melt by using a stirring tool until the reduced graphene oxide @ copper powder is blown. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 380 ℃, the temperature is kept for 3 hours, and the extrusion ratio is 24: 1, extrusion rate is 3.0mm/min, and finally solid solution treatment and aging treatment are carried out, wherein the solid solution temperature is 590 ℃, and the heat preservation time is 4 hours; the aging temperature is 380 ℃, and the heat preservation time is 24h, so as to obtain the aluminum matrix composite material.
Example 6
Alloy components: by taking the mass of the alloy as 100%, the reduced graphene oxide is 0.07%, the Zr is 0.16%, the Er is 0.08%, the Ti is 0.009%, the Fe is 0.068%, the Si is less than or equal to 0.047%, the rest elements are less than or equal to 0.01% each, and the balance is Al.
The preparation process and the proportion of the reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the volume ratio of alcohol to water is 1:12, KH-550 is contained in the solution in an amount of 0.4 vol.%, and is statically dissolved for 8 hours; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.4g/L, adding nano copper powder for ultrasonic treatment for 45min, wherein the particle size of the nano copper powder is 15nm, performing hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and sintering at 1200 ℃ for 2 hours to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 750 ℃, and Al-Er and Al-Zr intermediate alloy is added. And blowing the reduced graphene oxide @ copper powder into the aluminum melt by using argon, and fully stirring the melt by using a stirring tool until the reduced graphene oxide @ copper powder is blown. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 370 ℃, the temperature is kept for 5 hours, and the extrusion ratio is 30: 1, extruding at a speed of 4.0mm/min, and finally performing solid solution treatment and aging treatment, wherein the solid solution temperature is 585 ℃, and the heat preservation time is 4 hours; the aging temperature is 320 ℃, and the heat preservation time is 50h, so that the aluminum matrix composite material is obtained.
Comparative example 1 (without reduced graphene oxide @ copper and zirconium, erbium)
Alloy components: calculated by 100 percent of alloy mass, 0.073 percent of Fe, 0.032 percent of Si, less than or equal to 0.01 percent of each of the other elements and the balance of Al. Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, and the aluminum ingot is completely melted. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 400 ℃, the heat preservation is carried out for 3 hours, and the extrusion ratio is 20: 1, extruding at a speed of 4.0mm/min, and finally performing solid solution treatment and aging treatment at a solid solution temperature of 600 ℃ for 5 hours; the aging temperature is 400 ℃, and the heat preservation time is 48h, so that the aluminum-based material is obtained.
Comparative example 2 (without reduced graphene oxide @ copper)
Alloy components: calculated by the mass of the alloy as 100 percent, Zr 0.1 percent, Er 0.1 percent, Ti 0.009 percent, Fe 0.067 percent, Si 0.044 percent, and each of the other elements is less than or equal to 0.01 percent, and the balance is Al. Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 750 ℃, and Al-Er and Al-Zr intermediate alloy is added. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 400 ℃, the heat preservation is carried out for 3 hours, and the extrusion ratio is 20: 1, extruding at a speed of 4.0mm/min, and finally performing solid solution treatment and aging treatment at a solid solution temperature of 600 ℃ for 5 hours; the aging temperature is 400 ℃, and the heat preservation time is 48h, so that the aluminum-based material is obtained.
COMPARATIVE EXAMPLE 3 (without zirconium or erbium)
Alloy components: by taking the mass of the alloy as 100%, the reduced graphene oxide is 0.07%, the Fe is 0.067%, the Si is 0.032%, the Ti is 0.010%, and the balance is Al.
The preparation process and the proportion of the reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the ratio of alcohol to water is 3: 12, KH-550 is contained in the solution in an amount of 0.9 vol.%, and is statically dissolved for 4 hours; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.7g/L, adding nano copper powder for ultrasonic treatment for 50min, wherein the particle size of the nano copper powder is 30nm, carrying out hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and carrying out sintering at 1100 ℃ for 3 hours to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75%, reduced graphene oxide @ copper powder is blown into the aluminum melt by argon when the aluminum ingot is completely melted, and the melt is fully stirred by a stirring tool until the reduced graphene oxide @ copper powder is blown in. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 400 ℃, the heat preservation is carried out for 3 hours, and the extrusion ratio is 20: 1, extruding at a speed of 4.0mm/min, and finally performing solid solution treatment and aging treatment at a solid solution temperature of 600 ℃ for 5 hours; the aging temperature is 400 ℃, and the heat preservation time is 48h, so that the aluminum matrix composite material is obtained.
Comparative example 4 (lowering solution temperature and aging temperature)
Alloy components: by taking the mass of the alloy as 100%, the reduced graphene oxide is 0.05%, the Zr is 0.1%, the Er is 0.1%, the Ti is 0.009%, the Fe is 0.066%, the Si is 0.041%, the rest elements are less than or equal to 0.01% each, and the balance is Al.
The preparation process and the proportion of the pre-synthesized reduced graphene oxide @ copper are as follows: preparing a KH-550 silane coupling agent solution, wherein the ratio of alcohol to water is 7: 5, KH-550 is contained in the solution in an amount of 0.5 vol.%, and is statically dissolved for 6 hours; adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.5g/L, adding nano copper powder for ultrasonic treatment for 40min, wherein the particle size of the nano copper powder is 20nm, performing hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and performing sintering at 1000 ℃ for 3 hours to obtain the reduced graphene oxide @ copper composite powder.
Cleaning the furnace before opening the furnace, if the alloy except 1 series is produced, arranging a furnace washing to achieve the purpose of controlling the content of impurity elements, and adopting an aluminum ingot in a crane resistance furnace; the purity of the aluminum ingot is 99.75 percent, when the aluminum ingot is completely melted, the temperature of the aluminum melt is raised to 740 ℃, and Al-Er and Al-Zr intermediate alloy is added. And blowing the reduced graphene oxide @ copper powder into the aluminum melt by using argon, and fully stirring the melt by using a stirring tool until the reduced graphene oxide @ copper powder is blown. Blowing a 4AB type refining agent with the mass of 1.0 percent of the mass of the aluminum melt into the aluminum alloy by adopting argon; standing, keeping the temperature, slagging off, discharging at 720 ℃, and carrying out water-cooling semi-continuous casting ingot casting. Hoisting the ingot casting finished product out of the crystallizer, turning, cutting head and tail, turning surface oxide skin, and then performing extrusion deformation; the extrusion heating temperature is 350 ℃, the temperature is kept for 4 hours, and the extrusion ratio is 22: 1, extrusion rate is 3.0mm/min, and finally solid solution treatment and aging treatment are carried out, wherein the solid solution temperature is 500 ℃, and the heat preservation time is 4 hours; the aging temperature is 180 ℃, and the heat preservation time is 72h, so that the aluminum matrix composite material is obtained.
The materials of examples 1-6 and comparative examples 1-4 were subjected to tensile strength and conductivity tests under ambient conditions and at elevated temperature, the tensile strength tests being in accordance with GBT 228.1-2010 metal material tensile test part 1: the room temperature test method was performed, the conductivity test was performed according to the GBT 12966-.
TABLE 1
Comparing the comparative examples 1 and 2 with the examples 1 to 6, it can be known that the tensile strength and the conductivity of the material can be greatly increased by adding the reduced graphene oxide @ copper into the aluminum-based composite material, and the heat resistance of the tensile strength and the conductivity can be increased; comparing the comparative examples 2 and 3 with the examples 1 to 6, it can be seen that the addition of zirconium and erbium elements to the aluminum-based composite material can increase the tensile strength and the electrical conductivity of the material and also has the effect of increasing the heat resistance; furthermore, as can be seen from comparison of comparative example 4 with examples 1 to 6, the conditions for controlling the solution treatment and the aging treatment also have an effect of improving the tensile strength, the electrical conductivity and the heat resistance of the material.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. The preparation method of the aluminum matrix composite is characterized by comprising the following steps:
(1) charging an aluminum ingot into a furnace, and after the aluminum ingot is completely melted, preserving heat for 20-30min at the temperature of 710-;
(2) heating the aluminum melt to 740 ℃ and 760 ℃, adding Al-Er and Al-Zr intermediate alloy, and keeping the temperature of the melt for 10-30 min;
(3) blowing reduced graphene oxide @ copper powder into the aluminum melt by adopting argon, and stirring while blowing until the powder is blown in;
(4) blowing argon into a 4AB type refining agent, wherein the adding mass of the refining agent is 1.0-1.2% of the mass of the aluminum melt;
(5) keeping the temperature of the melt static for 8-10min, carrying out slagging-off treatment, discharging, and casting a cast ingot bar;
(6) cutting the head and the tail of the cast ingot, turning surface oxide skin, and then performing extrusion deformation;
(7) carrying out solid solution aging treatment on the extrusion piece to obtain a high-strength high-conductivity high-heat-resistance aluminum matrix composite;
wherein, the solid solution temperature in the step (7) is 560-; the aging temperature is 200-;
the aluminum-based composite material comprises the following alloy components, by mass, 0.01-0.09% of reduced graphene oxide, 0.05-0.2% of Zr, 0.05-0.2% of Er, 0.008-0.010% of Ti, less than or equal to 0.07% of Fe, less than or equal to 0.05% of Si, and the balance of Al.
2. The production method according to claim 1, wherein the mass percentage of each of the remaining elements in the aluminum-based composite material is 0.01% or less.
3. The preparation method according to claim 1, wherein the raw material for preparing the reduced graphene oxide @ copper in the step (3) comprises 1-10 layers of graphene oxide with a sheet diameter of 1-25 microns.
4. The preparation method of claim 1, wherein the reduced graphene oxide @ copper in the step (3) is prepared by:
preparing a KH-550 silane coupling agent solution, adding graphene oxide into the solution to enable the concentration of the graphene oxide to be 0.1-1g/L, adding nano copper powder for ultrasonic treatment for 30-60min, wherein the particle size of the nano copper powder is 5-30 nm, carrying out hydrogen reduction sintering on the obtained mixed solution after vacuum freeze drying treatment, and sintering at the temperature of 900-1200 ℃ for 1-5 hours to obtain reduced graphene oxide copper @ composite powder.
5. The preparation method according to claim 4, wherein the mass of copper in the reduced graphene oxide @ copper composite powder is 1.0-5.0%.
6. The method according to claim 4, wherein the KH-550 silane coupling agent solution is prepared by a method comprising: preparing a mixed solvent with the volume ratio of alcohol to water being 1-10:12-1, and dissolving KH-550 in the mixed solvent to obtain a KH-550 silane coupling agent solution, wherein the content of KH-550 in the silane coupling agent solution is 0.1-0.9 vol.%, and the standing dissolving time is 4-8 hours.
7. The preparation method according to claim 1, wherein the step (6) comprises an extrusion heating operation at a temperature of 300 ℃ to 400 ℃ for 3 to 5 hours at an extrusion ratio of 20 to 30: 1, extrusion rate 1.0-5.0 mm/min.
8. A high-strength, high-conductivity and high-heat-resistance aluminum-based composite material for splicing fittings, which is prepared by the preparation method of any one of claims 1 to 7.
9. A splicing fitting prepared from the high-strength high-conductivity high-heat-resistance aluminum-based composite material for the splicing fitting of claim 8.
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