CN113462918B - Preparation method of CNTs/Al-Li high-strength composite material - Google Patents
Preparation method of CNTs/Al-Li high-strength composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a CNTs/Al-Li high-strength composite material, which is implemented according to the following steps: 1. weighing an isopropanol solution, a zwitterionic dispersant, 2195 alloy powder, multi-wall CNTs and zirconia grinding balls, mixing the isopropanol solution and the zwitterionic dispersant, adding the multi-wall CNTs for ultrasonic dispersion, and finally mixing in a vibration powder mixer to obtain a CNTs solution; 2. adding 2195 alloy powder, zirconia grinding balls and CNTs solution into a ball-milling tank for ball milling, standing, and drying to obtain prefabricated powder B; 3. prepressing the prefabricated powder B, and then sintering to obtain a composite material C; 4. preheating the composite material C by using a muffle furnace, and then extruding by using an extruder to obtain a composite section D; 5. and carrying out solid solution treatment and aging treatment on the composite section D to obtain the CNTs/Al-Li high-strength composite material.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, and relates to a preparation method of a CNTs/Al-Li high-strength composite material.
Background
Aluminum alloy has high specific strength and rigidity and good corrosion resistance, and becomes an important arrow structure lightweight material. In order to meet the development requirements of a new generation of carrier rocket and improve the effective carrying capacity of the rocket, the light weight of rocket body structural parts is urgently needed to be realized. Meanwhile, the new generation of carrier rocket needs to realize generalization, combination and serialization of models to build a spectral series so as to adapt to the launching of different payloads. Therefore, the arrow-shaped structural part is required to have higher dimensional precision during forming so as to reduce manual trimming, improve production efficiency and meet the requirement of automatic assembly.
For high strength aluminum alloys, 2-series aluminum alloys based mainly on Al-Cu-Mg and 7-series aluminum alloys based mainly on Al-Zn-Mg-Cu are used. In the preparation of the aluminum-based composite material, the selection of the matrix can be pure aluminum, and various conventional aluminum alloys can also be adopted. In the current common industrial aluminum alloy, certain properties, such as Mg, Ni or Bi, Be, etc., can Be improved by adding specific metal elements to achieve the purpose of improving hardness or fluidity, and a mature industrial aluminum-based material system is formed. The system is divided into Al-Si, Al-Mg, Al-Li, Al-Fe, Al-Cu and the like. Compared with the conventional aluminum alloy, the aluminum-lithium alloy has lighter weight and higher strength, and the light weight of the arrow body structure part can be realized to a greater extent. Wherein 2195 aluminum-lithium alloy replaces 2219 aluminum alloy, which can improve the structural strength by 40 percent and reduce the mass by 10 percent. Nevertheless, the strength and elongation of the aluminum-lithium alloy still need to be further improved to expand the application ratio thereof in aerospace equipment.
Disclosure of Invention
The invention aims to provide a preparation method of a CNTs/Al-Li high-strength composite material, which solves the problem that the strength and the elongation of an aluminum-lithium alloy are poor in the prior art.
The technical scheme adopted by the invention is that the preparation method of the CNTs/Al-Li high-strength composite material is implemented according to the following steps:
step 1, weighing an isopropanol solution, a zwitterionic dispersant, 2195 alloy powder, multi-wall CNTs and zirconia grinding balls, adding the isopropanol solution and the zwitterionic dispersant into a container for mixing, then adding the multi-wall CNTs for ultrasonic dispersion, and finally placing the mixture into a vibration powder mixer for mixing to obtain the CNTs solution;
step 2, adding the 2195 alloy powder and zirconia grinding balls weighed in the step 1 and the CNTs solution obtained in the step 1 into a ball milling tank for ball milling, standing after ball milling, removing a suspension solution, and drying to obtain prefabricated powder B;
step 3, prepressing the prefabricated powder B obtained in the step 2 to obtain a prepressed blank, and sintering by adopting a rapid hot-pressing sintering furnace to obtain a composite material C;
step 4, preheating the composite material C obtained in the step 3 by using a muffle furnace, and then extruding the preheated composite material C by using an extruder to obtain an extruded composite section D;
and step 5, carrying out solid solution treatment and aging treatment on the composite section D to obtain the CNTs/Al-Li high-strength composite material.
The invention is also characterized in that:
the mass ratio of the multiwall CNTs, the zwitterionic dispersant and the isopropanol solution weighed in the step 1 is 0.5-1.5:0.1-2:100-200, the mass ratio of the isopropanol solution to the 2195 alloy powder is 1-1.5:1, and the mass ratio of the zirconia grinding balls to the 2195 alloy powder is 5-10: 1.
And (3) mixing in the container in the step 1 by using a magnetic stirrer, wherein the stirring time is 10-15 min.
The ultrasonic frequency of ultrasonic dispersion in the step 1 is 39-45KHz, and the time is 0.5-1 h; the vibration frequency of the vibration powder mixer is 40-50Hz, and the time is 0.5-1 h.
In the step 2, the ball milling rotation speed is 200-300r/min, the time is 2-4h, and the operation process of ball milling comprises the steps of firstly positively rotating for 10min, pausing for 10min and then reversely rotating for 10 min.
And (3) standing for 10-20min in the step (2), drying at 75-80 ℃ for 60-240min, and keeping the drying in the argon atmosphere.
In the step 3, the pre-pressing pressure is 8-12MPa, the time is 1-2min, the vacuum degree in the sintering process is 0-10Pa, the pressure is 30-50MPa, the temperature is raised at the heating rate of 100 ℃/min during sintering, the temperature is raised to 470 ℃ at 430 ℃ at the temperature of plus one material, the temperature is raised at the heating rate of 20 ℃/min, the temperature is maintained for 30-60min after the temperature is raised to 570 ℃ at 530 ℃ at the temperature of plus one material, and finally the composite material C is obtained after furnace cooling.
The preheating in the step 4 has the heating rate of 10-15 ℃/min, the heating to 370-plus-430 ℃, the heat preservation for 15-25min, the heating of the extrusion die of the extruder to 270-plus-300 ℃, the extrusion rate of 3-5mm/s and the extrusion ratio of 33: 1.
and 5, specifically, putting the composite section D obtained in the step 4 into a vacuum atmosphere furnace, heating to 440-plus-470 ℃ at the heating rate of 10-20 ℃/min, preserving heat for 0-10min, taking out the section, performing water quenching, cooling the furnace temperature to room temperature, putting the section into the furnace chamber again, heating to 190 ℃ at the heating rate of 10-20 ℃/min, preserving heat for 25-30h, taking out the section, and air cooling to obtain the CNTs/Al-Li high-strength composite material.
The invention has the beneficial effects that: according to the invention, CNTs are uniformly dispersed in 2195 alloy, so that the CNTs have higher strength (60-110 GPa) and rigidity and lower density (2.1 g/cm)3) And a larger aspect ratio (100 to 1000) and a higher heat conductivity (3000 to 6000W/m.K), thereby increasing the strength of the aluminum matrix and reducing the density, and further improving the weight reduction effect.
Drawings
FIG. 1 is a flow chart of the preparation method of a CNTs/Al-Li high-strength composite material of the invention;
FIG. 2 is a graph of the powder micro-topography of 20000 times that of the sample obtained in example 1 of the present invention;
FIG. 3 is a graph of the powder micro-topography of 20000 times that of the sample obtained in example 2 of the present invention;
FIG. 4 is a graph of the powder micro-topography of 20000 times that of the sample obtained in example 3 of the present invention;
FIG. 5 is a graph of the powder micro-topography of 20000 times the sample obtained in example 4 of the present invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention relates to a preparation method of a CNTs/Al-Li high-strength composite material, which is specifically implemented according to the following steps as shown in figure 1:
step 1, weighing an isopropanol solution, a zwitterionic dispersant, 2195 alloy powder, multi-wall CNTs and a zirconia grinding ball, wherein the mass ratio of the multi-wall CNTs to the zwitterionic dispersant to the isopropanol solution is 0.5-1.5:0.1-2:100-200, the mass ratio of the isopropanol solution to the 2195 alloy powder is 1-1.5:1, the mass ratio of the zirconia grinding ball to the 2195 alloy powder is 5-10:1, adding the isopropanol solution and the zwitterionic dispersant to a container for mixing, mixing by using a magnetic stirrer for 10-15min, then adding the multi-wall CNTs for ultrasonic dispersion, wherein the ultrasonic frequency of the ultrasonic dispersion is 39-45KHz, and the time is 0.5-1 h; the vibration frequency of the vibration powder mixer is 40-50Hz, the time is 0.5-1h, and finally the mixture is placed in the vibration powder mixer to be mixed to obtain CNTs solution;
step 2, adding the 2195 alloy powder and zirconia grinding balls weighed in the step 1 and the CNTs solution obtained in the step 1 into a ball milling tank for ball milling, wherein the ball milling rotation speed is 200-300r/min, the ball milling time is 2-4h, the ball milling operation process comprises the steps of positively rotating for 10min, pausing for 10min, then reversely rotating for 10min, standing after ball milling, the standing time is 10-20min, then removing the suspension solution, drying to obtain prefabricated powder B, wherein the drying temperature is 75-80 ℃, the drying time is 60-240min, and the drying is under the protection of argon atmosphere;
step 3, pre-pressing the prefabricated powder B obtained in the step 2 to obtain a pre-pressed blank, wherein the pre-pressed pressure is 8-12MPa, the time is 1-2min, then sintering is carried out by adopting a rapid hot-pressing sintering furnace, the vacuum degree in the sintering process is 0-10Pa, the pressure is 30-50MPa, the temperature is increased at the heating rate of 100 ℃/min firstly in the sintering process, the temperature is increased to 430 ℃ and 470 ℃, then the temperature is increased at the heating rate of 20 ℃/min, the temperature is maintained for 30-60min after the temperature is increased to 530 ℃ and 570 ℃, and finally, the composite material C is obtained by furnace cooling;
step 4, preheating the composite material C obtained in the step 3 by adopting a muffle furnace, wherein the preheating heating rate is 10-15 ℃/min, the temperature is increased to 430 ℃ for 370-plus-one times, the heat is preserved for 15-25min, an extrusion die of an extruder is heated to 300 ℃ for 270-plus-one times, then extruding the preheated composite material C by adopting the extruder, the extrusion rate is 3-5mm/s, and the extrusion ratio is 33: 1, obtaining an extruded composite section D;
and 5, carrying out solid solution treatment and aging treatment on the composite section D, specifically, putting the composite section D obtained in the step 4 into a vacuum atmosphere furnace, heating to 440-.
Example 1
The invention provides a preparation method of a CNTs/Al-Li high-strength composite material, which comprises the following steps:
step 1, preparing uniform CNTs solution
Weighing 60g of 2195 alloy powder, wherein the grain diameter of the alloy powder is 325 meshes (45 m), and weighing 300g of grinding balls, 240g of large balls and 60g of small balls, namely the ball-material ratio is 5:1, size-to-bead ratio 4: 1. adding 60g of isopropanol solution into a clean beaker, weighing 0.3g of zwitterionic dispersant (dodecyl dimethyl aminoethylenolactone), adding the dispersant into the isopropanol solution, stirring for 10min by using a magnetic stirrer, weighing 0.3g of CNTs (carbon nanotubes) in mass fraction after the dispersant is fully dissolved, wherein the CNTs are multi-walled CNTs, the pipe diameter of which is about 30-50nm, adding the CNTs into the well-dispersed solution, sealing the opening of the beaker by using a preservative film to prevent the solution from volatilizing, putting the solution into an ultrasonic machine, ultrasonically vibrating for 1h at the ultrasonic frequency of 40KHz, transferring the solution into a special bottle for a vibration powder mixing machine after the ultrasonic vibration is finished, and simultaneously adding 5 ZrO (zirconium dioxide) with the diameter of 10mm into the special bottle2And grinding balls are arranged on the vibration powder mixer, and the uniform CNTs solution A is obtained by vibrating for 30min at the vibration frequency of 40 Hz.
Step 2, wet ball milling
Adding the uniform CNTs solution A prepared in the step 1 and alloy powder into a ball milling tank which is ZrO2The material is ball-milling pot with diameter of 120mm, and then 300g ZrO is added2Grinding balls, wherein the ratio of big balls to small balls is 4: 1, namely 240g of big ball and 60g of small ball. Sealing the ball milling tank and introducing argon for atmosphere protectionTo prevent oxidation of the sample during ball milling. And mounting the ball milling tank on a ball mill, setting ball milling parameters, setting the ball milling rotation speed to be 200r/min, setting the ball milling time to be 4h, and setting the operation mode to be forward rotation for 10min, pause for 10min and reverse rotation for 10 min. Standing for 10min after the ball milling is finished, and sucking the suspension solution containing the residual CNTs at the upper layer by using a rubber head dropper. And taking out the ball-milled slurry, placing the ball-milled slurry into a culture dish, placing the culture dish into a vacuum oven, washing the vacuum oven with argon gas to ensure that the vacuum oven is completely in an argon atmosphere state, setting the drying temperature to be 80 ℃, and regularly drying for 2 hours. And taking out the powder after drying, putting the powder into a screening net for screening, and taking out the grinding balls to obtain the residual powder which is the prefabricated powder.
Step 3, rapid hot-pressing sintering
And (3) sintering the ball-milled powder obtained in the step (2) by using a rapid hot-pressing sintering furnace. Cutting graphite paper according to a sintering mould with the diameter of phi 40, paving the graphite paper in a graphite mould, pouring the powder obtained in the step two into the graphite mould, stacking the graphite paper, pressing the graphite paper by using a pressing head, and then pre-pressing the graphite paper by using a manual hydraulic press, wherein the pressure is 10MPa, and the pressure maintaining time is 1 min. And after the powder is filled into a graphite die, the graphite die is installed on a rapid hot-pressing sintering furnace. Setting a sintering program, wherein the specific process is that the pressure is increased to 40MPa within 1min and then is maintained, the temperature is increased to 470 ℃ at the heating rate of 100 ℃/min, the temperature is increased to 570 ℃ at the heating rate of 20 ℃/min, the temperature is maintained for 60min, and then the cylindrical sintered blank with the diameter of 40mm and the height of 15mm is obtained through furnace cooling.
Step 4, hot extrusion
Setting a muffle furnace temperature controller, heating to 370 ℃ at a heating rate of 10 ℃/min, preheating the sintered blank before extrusion for 20min, simultaneously heating the temperature of an extrusion die to more than 300 ℃ in advance by using a heating sleeve, quickly placing the sintered blank into the extrusion die after preheating, and extruding at an extrusion speed of 3mm/s to obtain the extruded composite section. The head and tail of 100mm material are removed from the extruded section, and the middle part is the prefabricated section.
Step 5, heat treatment
The method comprises two steps of solution treatment and aging treatment, wherein a vacuum atmosphere furnace is used for the heat treatment. The specific operation is as follows: and (4) cutting a proper length of the section bar obtained in the step (4), putting the section bar into a vacuum atmosphere furnace, washing the furnace cavity with argon, and using the argon as protective atmosphere to prevent the sample from being oxidized in the heating process. Setting a heating program, firstly heating to 470 ℃ at the heating rate of 10 ℃/min, then keeping the temperature for 10min, taking out the sample, performing water quenching, and finishing the solution treatment. After the solution treatment is finished, the sample is put into a furnace chamber again after the furnace temperature is reduced to room temperature, the gas is washed by argon, a heating procedure is set, the temperature is increased to 150 ℃ at the same heating rate of 10 ℃/min, the temperature is kept for 25h, the sample is taken out and air-cooled, and the CNTs/Al-Li high-strength composite material is obtained. In the heating and heat preservation processes of the heat treatment, argon is needed to be introduced for atmosphere protection in the whole process so as to prevent the sample from being damaged by oxidation at high temperature.
The micro-morphology of the CNTs/Al-Li high-strength composite material powder prepared in the embodiment 1 of the invention is shown in FIG. 2, the addition amount of the CNTs of the enhanced phase is 0.5%, and meanwhile, the combination of the CNTs of the enhanced phase and the aluminum-lithium alloy matrix is good; measuring the density of the CNTs/Al-Li high-strength composite material by using an Archimedes drainage method; using an HBRV-187.5 electric Brookfield hardness tester, testing the Brinell hardness at a force of 32.16N and a pressure maintaining time of 30 s; measuring the tensile strength by using a universal mechanical property testing machine; the density, hardness and tensile strength of the CNTs/Al-Li high-strength composite material prepared in the embodiment 1 of the invention are detected by the method, and the density is 2.701g/cm3The hardness was 245.3HV and the tensile strength was 736.5 MPa.
Example 2
The invention provides a preparation method of a CNTs/Al-Li high-strength composite material, as shown in figure 1, which comprises the following steps:
step 1, preparing uniform CNTs solution
Weighing 60g of 2195 alloy powder, wherein the grain diameter of the alloy powder is 325 meshes (45 m), and weighing 300g of grinding balls, 240g of large balls and 60g of small balls, namely the ball-material ratio is 5:1, size-to-bead ratio 4: 1. adding 60g of isopropanol solution into a clean beaker, weighing 0.6g of zwitterionic dispersant (dodecyl dimethyl aminoethylectone), adding into the isopropanol solution, stirring for 10min with a magnetic stirrer to fully dissolve the dispersantThen, 0.6g of CNTs (carbon nanotubes) is weighed, CNTs are multi-wall CNTs with the pipe diameter of about 30-50nm, the CNTs are added into the well dispersed solution, the opening of a beaker is sealed by a preservative film to prevent the solution from volatilizing, the solution is put into an ultrasonic machine and is ultrasonically vibrated for 1h at the ultrasonic frequency of 40KHz, after that, the solution is transferred into a special bottle for a vibrating powder mixer, and 7 ZrO particles with the diameter of 10mm are added simultaneously2And grinding balls are arranged on the vibration powder mixer, and the uniform CNTs solution is obtained by vibrating for 30min at the vibration frequency of 40 Hz.
Step 2, wet ball milling
Adding the uniform CNTs solution prepared in the step 1 and 2195 alloy powder into a ball milling tank which is ZrO2The material is ball-milling pot with diameter of 120mm, and then 300g ZrO is added2Grinding balls, which are classified into large balls (d 10mm) and small balls (d 5mm), and have a large-to-small ball ratio of 4: 1, namely 240g of big ball and 60g of small ball. The ball milling tank is sealed and argon is introduced for atmosphere protection to prevent the sample from being oxidized in the ball milling process. And mounting the ball milling tank on a ball mill, setting ball milling parameters, setting the ball milling rotation speed to be 200r/min, setting the ball milling time to be 4h, and setting the operation mode to be forward rotation for 10min, pause for 10min and reverse rotation for 10 min. Standing for 15min after the ball milling is finished, and sucking the suspension solution containing the residual CNTs at the upper layer by using a rubber head dropper. And taking out the ball-milled slurry, placing the ball-milled slurry into a culture dish, placing the culture dish into a vacuum oven, washing the vacuum oven with argon gas to ensure that the vacuum oven is completely in an argon atmosphere state, setting the drying temperature to be 80 ℃, and regularly drying for 2 hours. And taking out the powder after drying, putting the powder into a screening net for screening, and taking out the grinding balls to obtain the residual powder which is the prefabricated powder.
Step 3, rapid hot-pressing sintering
And (3) sintering the ball-milled powder obtained in the step (2) by using a rapid hot-pressing sintering furnace. Cutting graphite paper according to a sintering mould with the diameter of phi 40, paving the graphite paper in a graphite mould, pouring the powder obtained in the step two into the graphite mould, stacking the graphite paper, pressing the graphite paper by using a pressing head, and then pre-pressing the graphite paper by using a manual hydraulic press, wherein the pressure is 10MPa, and the pressure maintaining time is 1 min. And after the powder is filled into a graphite die, the graphite die is installed on a rapid hot-pressing sintering furnace. Setting a sintering program, wherein the specific process is that the pressure is increased to 40MPa within 1min and then is maintained, the temperature is increased to 470 ℃ at the heating rate of 100 ℃/min, the temperature is increased to 570 ℃ at the heating rate of 20 ℃/min, the temperature is maintained for 60min, and then the cylindrical sintered blank with the diameter of 40mm and the height of 15mm is obtained through furnace cooling.
Step 4, hot extrusion
Setting a muffle furnace temperature controller, heating to 370 ℃ at a heating rate of 10 ℃/min, preheating the sintered blank before extrusion for 20min, simultaneously heating the temperature of an extrusion die to more than 300 ℃ in advance by using a heating sleeve, quickly placing the sintered blank into the extrusion die after preheating, and extruding at an extrusion speed of 3mm/s to obtain the extruded composite section. The head and tail of 100mm material are removed from the extruded section, and the middle part is the prefabricated section.
Step 5, heat treatment
The method comprises two steps of solution treatment and aging treatment, wherein a vacuum atmosphere furnace is used for the heat treatment. The specific operation is as follows: and (4) cutting a proper length of the section bar obtained in the step (4), putting the section bar into a vacuum atmosphere furnace, washing the furnace cavity with argon, and using the argon as protective atmosphere to prevent the sample from being oxidized in the heating process. Setting a heating program, firstly heating to 470 ℃ at the heating rate of 10 ℃/min, then keeping the temperature for 10min, taking out the sample, performing water quenching, and finishing the solution treatment. After the solution treatment is finished, the sample is put into a furnace chamber again after the furnace temperature is reduced to room temperature, the gas is washed by argon, a heating procedure is set, the temperature is increased to 150 ℃ at the same heating rate of 10 ℃/min, the temperature is kept for 25h, the sample is taken out and air-cooled, and the CNTs/Al-Li high-strength composite material is obtained. In the heating and heat preservation processes of the heat treatment, argon is needed to be introduced for atmosphere protection in the whole process so as to prevent the sample from being damaged by oxidation at high temperature.
The micro-morphology of the CNTs/Al-Li high-strength composite material powder prepared in the embodiment 2 of the invention is shown in FIG. 3, the addition amount of the CNTs of the enhanced phase is 1%, and the combination of the CNTs of the enhanced phase and the aluminum-lithium alloy matrix is good; measuring the density of the CNTs/Al-Li high-strength alloy by an Archimedes drainage method; using an HBRV-187.5 electric Brookfield hardness tester, testing the Brinell hardness at a force of 32.16N and a pressure maintaining time of 30 s; using universal mechanical property testMeasuring the tensile strength by a machine; the density, hardness and tensile strength of the CNTs/Al-Li high-strength composite material prepared in the embodiment 2 of the invention are detected by the method, and the density is 2.686g/cm3The hardness was 261.2HV, and the tensile strength was 623.4 MPa.
Example 3
The invention provides a preparation method of a CNTs/Al-Li high-strength composite material, which comprises the following steps:
step 1, preparing uniform CNTs solution
Weighing 60g of 2195 alloy powder, wherein the grain diameter of the alloy powder is 325 meshes (45 m), and weighing 300g of grinding balls, 240g of large balls and 60g of small balls, namely the ball-material ratio is 5:1, size-to-bead ratio 4: 1. adding 60g of isopropanol solution into a clean beaker, weighing 0.9g of zwitterionic dispersant (dodecyl dimethyl aminoethylenolactone), adding the dispersant into the isopropanol solution, stirring for 10min by using a magnetic stirrer, weighing 0.9g of CNTs (carbon nanotubes) in mass fraction after the dispersant is fully dissolved, wherein the CNTs are multi-walled CNTs, the pipe diameter of which is about 30-50nm, adding the CNTs into the well-dispersed solution, sealing the opening of the beaker by using a preservative film to prevent the solution from volatilizing, putting the solution into an ultrasonic machine, ultrasonically vibrating for 1h at the ultrasonic frequency of 40KHz, transferring the solution into a special bottle for a vibration powder mixing machine after the ultrasonic vibration is finished, and simultaneously adding 8 ZrO (zirconium dioxide) with the diameter of 10mm2And grinding balls are arranged on the vibration powder mixer, and the uniform CNTs solution is obtained by vibrating for 30min at the vibration frequency of 40 Hz.
Step 2, wet ball milling
Adding the uniform CNTs solution prepared in the step 1 and 2195 alloy powder into a ball milling tank which is ZrO2The material is ball-milling pot with diameter of 120mm, and then 300g ZrO is added2Grinding balls, wherein the ratio of big balls to small balls is 4: 1, namely 240g of big ball and 60g of small ball. The ball milling tank is sealed and argon is introduced for atmosphere protection to prevent the sample from being oxidized in the ball milling process. And mounting the ball milling tank on a ball mill, setting ball milling parameters, setting the ball milling rotation speed to be 200r/min, setting the ball milling time to be 4h, and setting the operation mode to be forward rotation for 10min, pause for 10min and reverse rotation for 10 min. Standing for 18min after the ball milling is finished, and sucking the suspension solution containing the residual CNTs at the upper layer by using a rubber head dropper. Taking out the ball-milled slurry and placing the ball-milled slurry in a containerAnd (3) placing the culture dish in a vacuum oven, washing the vacuum oven with argon gas to ensure that the vacuum oven is completely in an argon atmosphere state, setting the drying temperature to be 80 ℃, and regularly drying for 2 hours. And taking out the powder after drying, putting the powder into a screening net for screening, and taking out the grinding balls to obtain the residual powder which is the prefabricated powder.
Step 3, rapid hot-pressing sintering
And (3) sintering the ball-milled powder obtained in the step (2) by using a rapid hot-pressing sintering furnace. Cutting graphite paper according to a sintering mould with the diameter of phi 40, paving the graphite paper in a graphite mould, pouring the powder obtained in the step two into the graphite mould, stacking the graphite paper, pressing the graphite paper by using a pressing head, and then pre-pressing the graphite paper by using a manual hydraulic press, wherein the pressure is 10MPa, and the pressure maintaining time is 1 min. And after the powder is filled into a graphite die, the graphite die is installed on a rapid hot-pressing sintering furnace. Setting a sintering program, wherein the specific process is that the pressure is increased to 40MPa within 1min and then is maintained, the temperature is increased to 470 ℃ at the heating rate of 100 ℃/min, the temperature is increased to 570 ℃ at the heating rate of 20 ℃/min, the temperature is maintained for 30min, and then the cylindrical sintered blank with the diameter of 40mm and the height of 15mm is obtained through furnace cooling.
Step 4, hot extrusion
Setting a muffle furnace temperature controller, heating to 370 ℃ at a heating rate of 10 ℃/min, preheating the sintered blank before extrusion for 20min, simultaneously heating the temperature of an extrusion die to more than 300 ℃ in advance by using a heating sleeve, quickly placing the sintered blank into the extrusion die after preheating, and extruding at an extrusion speed of 3mm/s to obtain the extruded composite section. The head and tail of 100mm material are removed from the extruded section, and the middle part is the prefabricated section.
Step 5, heat treatment
The method comprises two steps of solution treatment and aging treatment, wherein a vacuum atmosphere furnace is used for the heat treatment. The specific operation is as follows: and (4) cutting a proper length of the section bar obtained in the step (4), putting the section bar into a vacuum atmosphere furnace, washing the furnace cavity with argon, and using the argon as protective atmosphere to prevent the sample from being oxidized in the heating process. Setting a heating program, firstly heating to 470 ℃ at the heating rate of 10 ℃/min, then keeping the temperature for 10min, taking out the sample, performing water quenching, and finishing the solution treatment. After the solution treatment is finished, the sample is put into a furnace chamber again after the furnace temperature is reduced to room temperature, the gas is washed by argon, a heating procedure is set, the temperature is increased to 150 ℃ at the same heating rate of 10 ℃/min, the temperature is kept for 25h, the sample is taken out and air-cooled, and the CNTs/Al-Li high-strength composite material is obtained. In the heating and heat preservation processes of the heat treatment, argon is needed to be introduced for atmosphere protection in the whole process so as to prevent the sample from being damaged by oxidation at high temperature.
The micro-morphology of the CNTs/Al-Li high-strength composite material powder prepared in the embodiment 3 of the invention is shown in FIG. 4, the addition amount of the CNTs of the enhanced phase is 1.5%, and the combination of the CNTs of the enhanced phase and the aluminum-lithium alloy matrix is good; measuring the density of the CNTs/Al-Li high-strength composite material by using an Archimedes drainage method; using an HBRV-187.5 electric Brookfield hardness tester, testing the Brinell hardness at a force of 32.16N and a pressure maintaining time of 30 s; measuring the tensile strength by using a universal mechanical property testing machine; the density, hardness and tensile strength of the CNTs/Al-Li high-strength composite material prepared in the embodiment 3 of the invention are detected by the method, and the density is 2.644g/cm3, the hardness is 196.3HV and the tensile strength is 534.9 MPa.
Example 4
The invention provides a preparation method of a CNTs/Al-Li high-strength composite material, which comprises the following steps:
step 1, preparing uniform CNTs solution
Weighing 60g of 2195 alloy powder, wherein the grain diameter of the alloy powder is 325 meshes (45 m), and weighing 300g of grinding balls, 240g of large balls and 60g of small balls, namely the ball-material ratio is 5:1, size-to-bead ratio 4: 1. adding 60g of isopropanol solution into a clean beaker, weighing 1.2g of zwitterionic dispersant (dodecyl dimethyl aminoethylenolactone), adding the dispersant into the isopropanol solution, stirring for 10min by using a magnetic stirrer, weighing 1.2g of CNTs (carbon nanotubes) in mass fraction after the dispersant is fully dissolved, wherein the CNTs are multi-walled CNTs, the pipe diameter of which is about 30-50nm, adding the CNTs into the well-dispersed solution, sealing the opening of the beaker by using a preservative film to prevent the solution from volatilizing, putting the solution into an ultrasonic machine, ultrasonically vibrating for 1h at the ultrasonic frequency of 40KHz, transferring the solution into a special bottle for a vibration powder mixing machine after the ultrasonic vibration is finished, and simultaneously adding 10 ZrO (zirconium dioxide) with the diameter of 10mm into the special bottle2And grinding balls are arranged on the vibration powder mixer, and the uniform CNTs solution is obtained by vibrating for 30min at the vibration frequency of 40 Hz.
Step 2, wet ball milling
Adding the uniform CNTs solution prepared in the step 1 and 2195 alloy powder into a ball milling tank which is ZrO2The material is ball-milling pot with diameter of 120mm, and then 300g ZrO is added2Grinding balls, wherein the ratio of big balls to small balls is 4: 1, namely 240g of big ball and 60g of small ball. The ball milling tank is sealed and argon is introduced for atmosphere protection to prevent the sample from being oxidized in the ball milling process. And mounting the ball milling tank on a ball mill, setting ball milling parameters, setting the ball milling rotation speed to be 200r/min, setting the ball milling time to be 4h, and setting the operation mode to be forward rotation for 10min, pause for 10min and reverse rotation for 10 min. Standing for 20min after the ball milling is finished, and sucking the suspension solution containing the residual CNTs at the upper layer by using a rubber head dropper. And taking out the ball-milled slurry, placing the ball-milled slurry into a culture dish, placing the culture dish into a vacuum oven, washing the vacuum oven with argon gas to ensure that the vacuum oven is completely in an argon atmosphere state, setting the drying temperature to be 80 ℃, and regularly drying for 2 hours. And taking out the powder after drying, putting the powder into a screening net for screening, and taking out the grinding balls to obtain the residual powder which is the prefabricated powder.
Step 3, rapid hot-pressing sintering
And (3) sintering the ball-milled powder obtained in the step (2) by using a rapid hot-pressing sintering furnace. Cutting graphite paper according to a sintering mould with the diameter of phi 40, paving the graphite paper in the graphite mould, pouring the powder obtained in the step two into the graphite mould, stacking the graphite paper, pressing the graphite paper by using a pressing head, and pre-pressing the graphite paper by using a manual hydraulic press, wherein the pressure is 10MPa, and the pressure maintaining time is 1 min. And after the powder is filled into a graphite die, the graphite die is installed on a rapid hot-pressing sintering furnace. Setting a sintering procedure, wherein the specific process is that the pressure is increased to 40MPa within 1min and then is maintained, and the sintering procedure is carried out
Heating to 470 ℃ at a heating rate of 100 ℃/min, adjusting the heating rate to 20 ℃/min, heating to 530 ℃, keeping the temperature for 30min, and then cooling along with the furnace to obtain a cylindrical sintered blank with the diameter of 40mm and the height of 15 mm.
Step 4, hot extrusion
Setting a muffle furnace temperature controller, heating to 370 ℃ at a heating rate of 10 ℃/min, preheating the sintered blank before extrusion for 20min, simultaneously heating the temperature of an extrusion die to more than 300 ℃ in advance by using a heating sleeve, quickly placing the sintered blank into the extrusion die after preheating, and extruding at an extrusion speed of 3mm/s to obtain the extruded composite section. The head and tail of 100mm material are removed from the extruded section, and the middle part is the prefabricated section.
Step 5, heat treatment
The method comprises two steps of solution treatment and aging treatment, wherein a vacuum atmosphere furnace is used for the heat treatment. The specific operation is as follows: and (4) cutting a proper length of the section bar obtained in the step (4), putting the section bar into a vacuum atmosphere furnace, washing the furnace cavity with argon, and using the argon as protective atmosphere to prevent the sample from being oxidized in the heating process. Setting a heating program, firstly heating to 470 ℃ at a heating rate of 10 ℃/min, then keeping the temperature for 30min, taking out the sample, performing water quenching, and finishing the solution treatment. After the solution treatment is finished, the sample is put into a furnace chamber again after the furnace temperature is reduced to room temperature, the gas is washed by argon, a heating procedure is set, the temperature is increased to 150 ℃ at the same heating rate of 10 ℃/min, the temperature is kept for 25h, the sample is taken out and air-cooled, and the CNTs/Al-Li high-strength composite material is obtained. In the heating and heat preservation processes of the heat treatment, argon is needed to be introduced for atmosphere protection in the whole process so as to prevent the sample from being damaged by oxidation at high temperature.
The micro-morphology of the CNTs/Al-Li high-strength composite material powder prepared in the embodiment 4 of the invention is shown in FIG. 5, the addition amount of the CNTs of the enhanced phase is 2%, and the combination of the CNTs of the enhanced phase and the aluminum-lithium alloy matrix is good; measuring the density of the CNTs/Al-Li high-strength alloy by an Archimedes drainage method; using an HBRV-187.5 electric Brookfield hardness tester, testing the Brinell hardness at a force of 32.16N and a pressure maintaining time of 30 s; measuring the tensile strength by using a universal mechanical property testing machine; the density, hardness and tensile strength of the CNTs/Al-Li high-strength composite material prepared in the embodiment 4 of the invention are detected by the method, and the density of the CNTs/Al-Li high-strength composite material is 2.636g/cm3The hardness was 156.2HV, and the tensile strength was 446.3 MPa.
The properties of the high-strength composite material prepared by the invention are further illustrated by tests.
Four samples were taken:
firstly, the CNTs/Al-Li high-strength composite material prepared in the embodiment 1 is a sample 1;
(II) the difference from the embodiment 1 of the invention is only that the mass of CNTs weighed in the step 1 is 0.6g, the number of grinding balls added in the step 2 is 7, and the standing time after the ball grinding in the step 3 is finished is 15min, other contents are the same as those of the embodiment 1 of the invention, and are not described herein again, and the prepared CNTs/Al-Li high-strength composite material is the sample 2;
(III) the difference from the embodiment 1 of the invention is only that the mass of CNTs weighed in the step 1 is 0.9g, the number of grinding balls added in the step 2 is 8, and the standing time after the ball grinding in the step 3 is finished is 18min, other contents are the same as those in the embodiment 1 of the invention, and are not described herein again, and the prepared CNTs/Al-Li high-strength composite material is the sample 3;
(IV) the difference from the embodiment 1 of the invention is only that the mass of CNTs weighed in the step 1 is 1.2g, the number of grinding balls added in the step 2 is 10, and the standing time after the ball grinding in the step 3 is finished is 20min, other contents are the same as those of the embodiment 1 of the invention, and are not described herein again, and the prepared CNTs/Al-Li high-strength composite material is a sample 4;
measuring the density of the high-strength alloy by adopting an Archimedes drainage method; using an HBRV-187.5 electric Brookfield hardness tester, testing the Brinell hardness at a force of 32.16N and a pressure maintaining time of 30 s; the tensile strength is measured by using a universal mechanical property tester. The density, hardness and tensile strength of the four samples are detected, and the detection results are as follows:
as can be seen from the table, as the content of CNTs increases, the density tends to decrease, on one hand, because CNTs have a lower density than Al-Li alloy, and on the other hand, because the CNTs are agglomerated after the content is too high, the sintering property is deteriorated, which is also a cause of the decrease of tensile strength. In comparison, the hardness increases and then decreases due to the difference in deformation behavior of the composite material during compression and tension. Finally, the sample 1 is preferably selected as the best result of the experiment, and when the content of the CNTs is 0.5%, the mechanical property reaches the best.
Claims (3)
1. A preparation method of a CNTs/Al-Li high-strength composite material is characterized by comprising the following steps:
step 1, weighing an isopropanol solution, a zwitterionic dispersant, 2195 alloy powder, multi-wall CNTs and zirconia grinding balls, adding the isopropanol solution and the zwitterionic dispersant into a container, stirring for 10-15min by using a magnetic stirrer, then adding the multi-wall CNTs, performing ultrasonic dispersion at an ultrasonic frequency of 39-45KHz for 0.5-1h, and finally placing the mixture into a vibration powder mixer, and mixing for 0.5-1h at a vibration frequency of 40-50Hz to obtain the CNTs solution;
the mass ratio of the weighed multiwall CNTs, the zwitterionic dispersant and the isopropanol solution is 0.5-1.5:0.1-2:100-200, the mass ratio of the isopropanol solution to the 2195 alloy powder is 1-1.5:1, and the mass ratio of the zirconia grinding balls to the 2195 alloy powder is 5-10: 1;
step 2, adding the 2195 alloy powder and zirconia grinding balls weighed in the step 1 and the CNTs solution obtained in the step 1 into a ball milling tank for ball milling, standing after ball milling, removing a suspension solution, and drying to obtain prefabricated powder B;
wherein, the ball milling conditions are as follows: the ball milling rotation speed is 200-300r/min, the time is 2-4h, the ball milling operation process comprises forward rotation for 10min, pause for 10min and then reverse rotation for 10 min; standing for 10-20min, drying at 75-80 deg.C for 60-240min under the protection of argon atmosphere;
step 3, prepressing the prefabricated powder B obtained in the step 2 to obtain a prepressed blank, and sintering by adopting a rapid hot-pressing sintering furnace to obtain a composite material C;
step 4, preheating the composite material C obtained in the step 3 by using a muffle furnace, and then extruding the preheated composite material C by using an extruder to obtain an extruded composite section D;
step 5, carrying out solid solution treatment and aging treatment on the composite section D to obtain a CNTs/Al-Li high-strength composite material;
and specifically, putting the composite section D obtained in the step 4 into a vacuum atmosphere furnace, heating to 440-plus-470 ℃ at the heating rate of 10-20 ℃/min, preserving the temperature for 0-10min, taking out the section, performing water quenching, putting the section into the furnace chamber again after the furnace temperature is reduced to room temperature, heating to 130-plus-190 ℃ at the heating rate of 10-20 ℃/min, preserving the temperature for 25-30h, taking out the section, and air cooling to obtain the CNTs/Al-Li high-strength composite material.
2. The method for preparing a CNTs/Al-Li high-strength composite material according to claim 1, wherein the pre-pressing pressure in step 3 is 8-12MPa, the time is 1-2min, the vacuum degree in the sintering process is 0-10Pa, the pressure is 30-50MPa, the temperature is raised at a rate of 100 ℃/min during sintering, the temperature is raised to 470 ℃ at 430 ℃ and then at a rate of 20 ℃/min, the temperature is maintained for 30-60min after the temperature is raised to 570 ℃ at 530 ℃ and the like, and finally the composite material C is obtained after furnace cooling.
3. The method for preparing a CNTs/Al-Li high-strength composite material according to claim 1, wherein the preheating in step 4 is performed at a heating rate of 10-15 ℃/min, at a temperature of 430 ℃ for 370 ℃ and at a temperature for 15-25min, and the extrusion mold of an extruder is heated at a temperature of 300 ℃ for 270 ℃ and at an extrusion rate of 3-5mm/s, and the extrusion ratio is 33: 1.
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