CN115780801A - Preparation method of ball-milled carbon nanotube modified aluminum-based composite material at high temperature - Google Patents
Preparation method of ball-milled carbon nanotube modified aluminum-based composite material at high temperature Download PDFInfo
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- CN115780801A CN115780801A CN202211425031.2A CN202211425031A CN115780801A CN 115780801 A CN115780801 A CN 115780801A CN 202211425031 A CN202211425031 A CN 202211425031A CN 115780801 A CN115780801 A CN 115780801A
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Abstract
The invention discloses a preparation method of a ground carbon nanotube modified aluminum matrix composite, which is characterized by comprising the following steps: step 1: premixing the carbon nano tube and copper powder to form a prefabricated body of the carbon nano tube and the copper; step 2: placing the prefabricated body of the carbon nano tube and the copper and an aluminum ingot into a ball milling tank, heating the ball milling tank, and placing ball milling beads into the ball milling tank; and step 3: and (3) carrying out ball milling on the prefabricated body of the carbon nano tube and the copper, the aluminum ingot and the ball milling beads in a ball milling tank for a preset time at a preset rotating speed, filtering a ball milling product in a preset temperature environment after the ball milling is finished, and screening out the ball milling beads to obtain the carbon nano tube milled modified aluminum-based composite material. The traditional powder metallurgy and the stirring casting are combined into one, so that the production efficiency is greatly improved, and the method has higher practical production guiding significance.
Description
Technical Field
The invention relates to the technical field of aluminum alloy preparation, in particular to a preparation method of a ball-milled carbon nanotube modified aluminum matrix composite material at a high temperature.
Background
Aluminum and aluminum alloy have excellent properties such as light weight, corrosion resistance, good heat conductivity and electric conductivity, become key materials in national important fields such as aerospace, transportation and the like, and are widely applied to important parts such as main structures of aircrafts, skins, automobile structures and the like. Since the discovery of Carbon Nanotubes (CNTs) in 1991, due to the existence of special carbon atom sp2 hybridization in the structure, the Carbon Nanotubes (CNTs) have the characteristics of low density, high specific surface area, large length-diameter ratio, excellent electric and heat conductivity, ultrahigh tensile strength (60 GPa), ultrahigh elastic modulus (1 TPa) and the like, are ideal reinforcements of metal-based composite materials, and have attracted wide attention of scholars at home and abroad. However, although the high-performance aluminum-based composite material can be prepared by the traditional powder metallurgy process, the process flow is long; the stirring casting process with high production efficiency cannot prepare high-performance materials due to the density difference between the carbon nano tube and the aluminum.
Chinese patent publication No. CN109020590B discloses a method for preparing a carbon nanotube reinforced alumina-based composite material by using a spray pyrolysis hot pressing method, and belongs to the technical field of composite material preparation. Adding pretreated carbon nanotubes and sodium dodecyl sulfate into deionized water to prepare a carbon nanotube dispersion liquid, adding aluminum nitrate to prepare a carbon nanotube/aluminum salt solution, adding ammonia water to generate a carbon nanotube/aluminum hydroxide sol, atomizing the carbon nanotube/aluminum hydroxide sol into small droplets, evaporating the moisture of the droplets in a short time through a pyrolysis furnace, decomposing the aluminum hydroxide into amorphous alumina, coating the carbon nanotubes uniformly dispersed in the droplets to obtain amorphous alumina-coated carbon nanotube spherical particles with uniform particle size, and performing hot-pressing sintering on the spherical powder to generate the carbon nanotube reinforced alumina-based composite material. However, the method has complex process and is not suitable for mass production. Chinese patent publication No. CN110938764B discloses a method for preparing a carbon nanotube/aluminum composite material with high mechanical strength and high conductivity, comprising the following steps: the method comprises the following steps: taking a single-walled carbon nanotube with the tube diameter of less than 6nm, and etching the cap end of the carbon nanotube at high temperature by using an etching agent to obtain the single-walled carbon nanotube with an open tail end; step two: the end opening single-wall carbon nano tube with the length-diameter ratio of about 250 is obtained by controlling the ball milling time or the carbon nano tube growth time. The surface of the single-walled carbon nanotube is plated with a boride or rare earth plating layer with excellent wettability with an aluminum matrix, so that the compatibility of the single-walled carbon nanotube with the aluminum matrix is improved, the single-walled carbon nanotube is uniformly distributed in the aluminum matrix, and meanwhile, the high-temperature annealing treatment increases the diffusion of metal atoms and the like among carbon tubes, so that the overall mechanical property and the conductivity of the carbon nanotube aluminum composite material are effectively improved. However, the method needs an etchant to etch the cap end of the carbon nanotube at a high temperature, and the fault tolerance is low.
Therefore, a simple and efficient preparation method of the carbon nanotube modified aluminum matrix composite material is still lacking at present.
Disclosure of Invention
The invention aims to provide a preparation method of a ball-milled carbon nanotube modified aluminum-based composite material at high temperature. The method combines the traditional powder metallurgy and stirring casting into a whole, shortens the process flow, greatly improves the production efficiency and has higher practical production guiding significance.
In order to realize the purpose, the preparation method of the milled carbon nanotube modified aluminum matrix composite material comprises the following steps:
step 1: the carbon nano tube and copper powder are premixed to form a prefabricated body of the carbon nano tube and copper, and the surface of the carbon nano tube is coated with a layer of copper to increase the wettability with an aluminum matrix;
step 2: the carbon nano tube and copper prefabricated body and the aluminum ingot are placed in a ball milling tank, the ball milling tank is heated, and ball milling beads are placed in the ball milling tank, the ball milling tank of the traditional planetary ball mill is additionally provided with a heating function, the temperature can be raised to a temperature above the liquidus line of aluminum, and the aluminum can be melted;
and step 3: the method comprises the following steps of carrying out ball milling on a prefabricated body of the carbon nano tube and the copper, an aluminum ingot and ball milling beads in a ball milling tank at a preset rotating speed for a preset time, filtering ball milling products in a preset temperature environment after the ball milling is finished, screening out the ball milling beads to obtain the modified aluminum-based composite material for milling the carbon nano tube, wherein the designed carbon nano tube is uniformly dispersed in aluminum liquid, the aluminum liquid and the ball milling beads in the ball milling tank are poured on a sieve made of a steel wire mesh under a high-temperature environment, the aluminum liquid flows through the sieve, and the ball milling beads are left on the sieve, so that a filtering effect is achieved.
In the step 1 of the technical scheme, the carbon nano tube and the copper powder are premixed by a high-speed shearing machine, and the rotating speed of the high-speed shearing machine is 1000-5000 r/min. The carbon nano tube and the copper powder can not be tightly combined when the rotating speed is lower than 1000r/min, and the structure of the carbon nano tube can be damaged when the rotating speed is higher than 5000r/min.
In step 1 of the above technical scheme, the mass percent of the carbon nanotubes in the preform of carbon nanotubes and copper is 1 to 20wt.%. Below 1wt.% the strengthening effect will not be achieved, above 20wt.% the copper will not form an effective wetting layer.
In step 2 of the above technical solution, the mass of the preform of carbon nanotube and copper is 1-10 wt.% of the total mass of the preform of carbon nanotube and copper and the aluminum ingot. A mass percentage of less than 1wt.% will not provide a strengthening effect, a mass percentage of more than 10wt.% will make it difficult to disperse the preform in the matrix.
In the step 2 of the above technical scheme, the heating temperature for heating the ball milling tank is 500-800 ℃. The aluminum liquid is solidified at the temperature lower than 500 ℃, and the carbon nano tube is ablated when the temperature is higher than 800 ℃.
In the step 2 of the technical scheme, the mass of the ball milling beads is 9-11 times of that of the ball milling material.
In the step 3 of the technical scheme, the rotating speed of the ball milling treatment in the ball milling tank is 100-2000 r/min. The carbon nano tube can not be uniformly dispersed in the aluminum liquid when the rotating speed is lower than 100r/min, and the structure of the carbon nano tube can be damaged when the rotating speed is higher than 2000r/min
In the step 3 of the technical scheme, the ball milling treatment time in the ball milling tank is 0.5-10 h.
In the step 3 of the technical scheme, after the ball milling is finished, the ball milling product is filtered at the temperature of 500-800 ℃. The aluminum liquid is solidified at the temperature lower than 500 ℃, and the carbon nano tube is ablated when the temperature is higher than 800 ℃.
In step 3 of the above technical scheme, after the ball milling is finished, the ball milled product is filtered by using a filter sieve made of a steel wire mesh. With other filter screens ablation may occur and introduce impurities.
The invention has the beneficial effects that:
the method improves the interface combination of the carbon nano tube and the aluminum liquid through the pre-combination of the copper powder and the carbon nano tube;
at present, the industry needs to prepare a preform by powder metallurgy, and then melt the preform after the powder metallurgy into a base material by adopting a high-temperature melting mode. The invention is equivalent to ball milling while smelting, which can not only reduce the structural damage of the carbon nano tube caused by mechanical ball milling impact by using the resistance of aluminum liquid, but also enable the additives during stirring and smelting to be uniformly dispersed in the matrix. The traditional powder metallurgy and stirring casting are combined into a whole, the technical advantages of the traditional powder metallurgy and stirring casting are fully exerted, and the superior performance of the material is ensured while the preparation efficiency is greatly improved;
the raw materials used in the invention are green and environment-friendly, the process operation is simple, and the method is suitable for large-scale industrial production.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
A preparation method of a ball-milled carbon nanotube modified aluminum matrix composite material at a high temperature comprises the following steps:
step 1: and premixing the carbon nano tube and the copper powder by adopting a high-speed shearing machine at the rotating speed of 3000r/min to form a prefabricated body of the carbon nano tube and the copper, wherein the mass fraction of the carbon nano tube is 5wt.%.
Step 2: placing a prefabricated body of carbon nano tubes and copper and an aluminum ingot in a ball milling tank, heating the ball milling tank at 700 ℃, and placing ball milling beads with ten times of the mass of ball milling materials, wherein the prefabricated body of the carbon nano tubes and the copper accounts for 2 wt% of the total mass of the prefabricated body of the carbon nano tubes and the copper and the aluminum ingot.
And step 3: and (3) performing ball milling on the prefabricated body of the carbon nano tube and the copper, the aluminum ingot and the ball milling beads in a ball milling tank at the rotating speed of 1000r/min for 3h, filtering a ball milling product at the temperature of 600 ℃ after the ball milling is finished, and screening out the ball milling beads to obtain the carbon nano tube milled modified aluminum-based composite material.
Example 2
The preparation is carried out according to the steps of the embodiment 1, and the difference from the embodiment 1 is that the rotating speed of the high-speed shearing machine in the step 1 is 1000r/min.
Example 3
The preparation is carried out according to the steps of the embodiment 1, and the difference from the embodiment 1 is that the rotating speed of the high-speed shearing machine in the step 1 is 2000r/min.
Example 4
The preparation method is carried out according to the steps of the embodiment 1, and the difference from the embodiment 1 is that the rotating speed of the high-speed shearing machine in the step 1 is 4000r/min.
Example 5
Prepared according to the procedure of example 1, except that the carbon nanotubes in the procedure of example 1 are 1wt.% in terms of the mass percentage of the preform of carbon nanotubes and copper.
Example 6
Prepared according to the procedure of example 1, except for the difference from example 1 that the carbon nanotubes in the procedure of step 1 are 10wt.% in terms of the mass percentage of the preform of carbon nanotubes and copper.
Example 7
Prepared according to the procedure of example 1, except that the carbon nanotubes in the procedure of example 1 are 15wt.% in terms of the mass percentage of the preform of carbon nanotubes and copper.
Example 8
Prepared according to the procedure of example 1, except for the difference from example 1 in that the preform of carbon nanotubes and copper in the step 2 accounts for 1wt.% of the total mass of the preform of carbon nanotubes and copper and the aluminum ingot.
Example 9
Prepared according to the procedure of example 1, except for the difference from example 1 in that the preform of carbon nanotubes and copper in the step 2 accounts for 3wt.% of the total mass of the preform of carbon nanotubes and copper and the aluminum ingot.
Example 10
Prepared according to the procedure of example 1, except for the difference from example 1 in that the preform of carbon nanotubes and copper in the procedure of step 2 accounts for 4wt.% of the total mass of the preform of carbon nanotubes and copper and the aluminum ingot.
Example 11
The preparation was carried out by following the procedure of example 1, except that the heating temperature to the ball milling pot in said step 2 was 500 ℃.
Example 12
The preparation was carried out by following the procedure of example 1, differing from example 1 in that the heating temperature to the ball milling pot in said step 2 was 600 ℃.
Example 13
The preparation was carried out by following the procedure of example 1, differing from example 1 in that the heating temperature to the ball milling pot in said step 2 was 800 ℃.
Example 14
The preparation was carried out by following the procedure of example 1, and the difference from example 1 was that the rotation speed of the ball mill in the step 3 was 100r/min.
Example 15
The preparation was carried out by following the procedure of example 1, except that the rotation speed of the ball mill in the step 3 was 500r/min.
Example 16
The preparation was carried out by following the procedure of example 1, and the difference from example 1 was that the rotation speed of the ball mill in the step 3 was 1500r/min.
Example 17
Prepared according to the procedure of example 1, except that the ball milling time in the step 3 is 0.5h in example 1.
Example 18
Prepared according to the procedure of example 1, except that the ball milling time in the step 3 was 6 hours in example 1.
Example 19
Prepared according to the procedure of example 1, except that the ball milling time in the step 3 is 9 hours from the example 1.
The tensile strength and elongation of the carbon nanotube-reinforced aluminum matrix composite obtained in examples 1 to 19 were measured, and the results are shown in table 1.
TABLE 1 comparison of the mechanical properties of examples 1 to 19
| Sample (I) | Axial tensile strength MPa | Axial elongation (%) |
| Example 1 | 585 | 7.1 |
| Example 2 | 432 | 7.2 |
| Example 3 | 514 | 8.1 |
| Example 4 | 532 | 8.0 |
| Example 5 | 539 | 7.8 |
| Example 6 | 552 | 7.1 |
| Example 7 | 473 | 7.2 |
| Example 8 | 489 | 8.1 |
| Example 9 | 555 | 8.0 |
| Example 10 | 538 | 7.8 |
| Example 11 | 528 | 7.5 |
| Example 12 | 514 | 7.3 |
| Example 13 | 473 | 6.9 |
| Example 14 | 489 | 7.5 |
| Example 15 | 546 | 7.3 |
| Example 16 | 575 | 7.1 |
| Example 17 | 523 | 7.2 |
| Example 18 | 546 | 7.3 |
| Example 19 | 549 | 7.5 |
As can be seen from the data in table 1, from the rotational speed of the high-speed shearing machine, the mass percentage of the carbon nanotube in the carbon nanotube-copper preform, the total mass ratio of the carbon nanotube-copper preform in the preform-aluminum ingot, the heating temperature of the ball milling tank, the rotational speed of the ball milling, the ball milling time and other 6 process parameters, an orthogonal test is performed, and mechanical property tests show that the rotational speed of the high-speed shearing machine adopted in example 1 is 3000r/min, the mass percentage of the carbon nanotube in the carbon nanotube-copper preform is 5wt.%, the total mass ratio of the carbon nanotube-copper preform in the preform-aluminum ingot is 2wt.%, the heating temperature of the ball milling tank is 700 ℃, the rotational speed of the ball milling is 1000r/min, and the ball milling time is 3 hours, so that the tensile strength of the prepared aluminum-based composite material reaches 585MPa, and the elongation reaches 7.1%.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (10)
1. A preparation method of a ball-milled carbon nanotube modified aluminum matrix composite material at a high temperature is characterized by comprising the following steps:
step 1: premixing the carbon nano tube and copper powder to form a prefabricated body of the carbon nano tube and the copper;
step 2: placing the prefabricated body of the carbon nano tube and the copper and an aluminum ingot into a ball milling tank, heating the ball milling tank, and placing ball milling beads into the ball milling tank;
and step 3: and (3) carrying out ball milling on the prefabricated body of the carbon nano tube and the copper, the aluminum ingot and the ball milling beads in a ball milling tank for a preset time at a preset rotating speed, filtering a ball milling product in a preset temperature environment after the ball milling is finished, and screening out the ball milling beads to obtain the carbon nano tube milled modified aluminum-based composite material.
2. The method for preparing the ball-milled carbon nanotube modified aluminum matrix composite material at the high temperature according to claim 1, which is characterized in that: in the step 1, the carbon nano tubes and the copper powder are premixed by a high-speed shearing machine, and the rotating speed of the high-speed shearing machine is 1000-5000 r/min.
3. The method for preparing the ball-milled carbon nanotube modified aluminum matrix composite material at the high temperature according to claim 1, which is characterized in that: in the step 1, the mass percentage of the carbon nanotubes in the preform of carbon nanotubes and copper is 1 to 20wt.%.
4. The method for preparing the ball-milled carbon nanotube modified aluminum matrix composite material at the high temperature according to claim 1, which is characterized in that: in step 2, the carbon nanotube and copper preform accounts for 1-10 wt% of the total mass of the carbon nanotube and copper preform and the aluminum ingot.
5. The method for preparing a ball-milled carbon nanotube modified aluminum-based composite material at a high temperature according to claim 1, which is characterized in that: in the step 2, the heating temperature for heating the ball milling tank is 500-800 ℃.
6. The method for preparing the ball-milled carbon nanotube modified aluminum matrix composite material at the high temperature according to claim 1, which is characterized in that: in the step 2, the mass of the ball milling beads is 9-11 times of that of the ball milling material.
7. The method for preparing the ball-milled carbon nanotube modified aluminum matrix composite material at the high temperature according to claim 1, which is characterized in that: in the step 3, the rotating speed of the ball milling treatment in the ball milling tank is 100-2000 r/min.
8. The method for preparing the ball-milled carbon nanotube modified aluminum matrix composite material at the high temperature according to claim 1, which is characterized in that: in the step 3, the ball milling treatment time in the ball milling tank is 0.5-10 h.
9. The method for preparing a ball-milled carbon nanotube modified aluminum-based composite material at a high temperature according to claim 1, which is characterized in that: in the step 3, after the ball milling is finished, filtering the ball milling product at the temperature of 500-800 ℃.
10. The method for preparing the ball-milled carbon nanotube modified aluminum matrix composite material at the high temperature according to claim 1, which is characterized in that: and in the step 3, filtering the ball-milled product by using a filter sieve made of a steel wire mesh after the ball milling is finished.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116116514A (en) * | 2023-04-13 | 2023-05-16 | 山东工业职业学院 | Preparation device and method of carbon nano tube composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116116514A (en) * | 2023-04-13 | 2023-05-16 | 山东工业职业学院 | Preparation device and method of carbon nano tube composite material |
| CN116116514B (en) * | 2023-04-13 | 2023-06-20 | 山东工业职业学院 | Preparation device and method of carbon nano tube composite material |
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