CN113136508A - High-strength plastic single-walled carbon nanotube aluminum-based composite material and preparation method thereof - Google Patents

High-strength plastic single-walled carbon nanotube aluminum-based composite material and preparation method thereof Download PDF

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CN113136508A
CN113136508A CN202110422450.XA CN202110422450A CN113136508A CN 113136508 A CN113136508 A CN 113136508A CN 202110422450 A CN202110422450 A CN 202110422450A CN 113136508 A CN113136508 A CN 113136508A
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aluminum
composite material
carbon nanotube
walled carbon
based composite
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徐文雷
刘爱军
万刚
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Suzhou Alome Science & Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium
    • C22C21/06Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08Alloys based on aluminium with magnesium as the next major constituent with silicon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/17Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
    • B22F3/172Continuous compaction, e.g. rotary hammering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/0408Light metal alloys
    • C22C1/0416Aluminium-based alloys
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/04Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)

Abstract

The invention provides a high-strength plastic single-walled carbon nanotube aluminum-based composite material, which comprises 0.05-0.4 wt% of single-walled carbon nanotubes and 99.6-99.95 wt% of aluminum matrix; the aluminum matrix is pre-alloyed powder of aluminum alloy, and the high-strength plastic aluminum matrix composite material is obtained by weighing single-walled carbon nanotubes and aluminum matrix raw materials, uniformly mixing the single-walled carbon nanotubes and the aluminum matrix raw materials in an ultrasonic dispersion manner, hot-pressing sintering and multi-directional forging rolling; the strength of the composite material is improved by using the single-walled carbon nanotube as a reinforcing phase, and the compactness and the strength of the aluminum matrix composite material are further improved by the preparation process and multidirectional forging, so that the aluminum matrix composite material has excellent comprehensive performance.

Description

High-strength plastic single-walled carbon nanotube aluminum-based composite material and preparation method thereof
Technical Field
The invention relates to the technical field of aluminum alloy matrix composite materials, in particular to a high-strength plastic single-walled carbon nanotube aluminum matrix composite material and a preparation method of the composite material.
Background
In the technical field of reinforced matrix composite materials, the aluminum alloy matrix composite material has the characteristics of high specific strength and specific modulus, low thermal expansion coefficient and good high-temperature performance, and has good fatigue resistance and wear resistance; meanwhile, the aluminum alloy matrix composite material has the advantages of wide selection range of the matrix, mature material processing technology, excellent plastic forming performance, good heat treatment performance and easy processing and preparation. Has become an important direction for the research and development of high-performance materials in aviation, aerospace and other advanced technical departments, and is also one of the hot spots for the research of new materials at home and abroad in recent years. Through the optimization design of the components, the content and the distribution of the matrix and the reinforcing phase of the aluminum alloy matrix composite material, specific mechanical properties and physical properties can be combined to meet the requirements of different product properties.
The 6061 aluminum alloy section belongs to 6-series Al-Si-Mg-series alloy, is a medium-high strength aluminum alloy which can be strengthened by heat treatment, and has the characteristics of light weight, high strength and good corrosion resistance, and simultaneously has good toughness, good welding performance and good machining performance. Meanwhile, the alloy still has good plasticity after annealing, and is widely applied to industries such as aerospace, automobile industry, aluminum products for packaging, architectural decoration, electronic home appliances and the like at present. The 6061 aluminum alloy can be used as a matrix of a high-strength high-plasticity aluminum-based composite material, and the single-walled carbon nanotube can improve the strength of the material. However, the single-walled carbon nanotube reinforced aluminum matrix composite has few commercial products, the preparation process is complex, and the comprehensive performance is difficult to control.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-strength plastic single-walled carbon nanotube aluminum-based composite material, wherein a single-walled carbon nanotube is used as a reinforcing part to reinforce the 6061 aluminum-based material, and the composite material is prepared by hot-pressing sintering and multidirectional forging to form the high-strength plastic single-walled carbon nanotube aluminum-based composite material; the method provides a new method and a new idea for preparing the high-performance aluminum-based composite material, which have stable performance and controllable process and can realize industrialization.
In order to achieve the above object, the present invention provides a high-strength plastic single-walled carbon nanotube aluminum matrix composite, comprising:
0.05-0.4 wt% of single-walled carbon nanotube and 99.6-99.95 wt% of aluminum matrix;
the aluminum substrate is 6061 aluminum alloy, and the 6061 aluminum alloy is pre-alloy powder.
The prealloying powder 6061 aluminum alloy comprises the following components:
Si:0.4~0.8wt%;
Zn:≤0.25wt%;
Cu:0.15~0.4wt%;
Mg:0.8~1.2wt%;
mn: less than or equal to 0.15 wt%; the balance being Al.
In order to realize the aim, the invention also provides a preparation method for preparing the high-strength plastic single-walled carbon nanotube aluminum-based composite material, which comprises the following steps:
s1, mixing the raw materials, and respectively weighing 0.05-0.4 wt% of the single-walled carbon nanotube and 99.6-99.95 wt% of the aluminum matrix pre-alloy powder as the raw materials; dispersing and mixing the weighed single-walled carbon nanotube and the aluminum matrix material uniformly in an ultrasonic wave to obtain mixed powder;
s2, carrying out hot-pressing sintering on the powder uniformly mixed in the step S1 to obtain an aluminum-based composite material blank of 6061 aluminum alloy;
and S3, multi-directional forging, namely, carrying out multi-directional forging processing on the aluminum-based composite material blank obtained in the step S2 to obtain the high-strength plastic aluminum-based composite material.
Preferably, the grain size of the pre-alloyed powder in the step S1 is 5-50 microns;
preferably, the ultrasonic dispersion time in the step S1 is 55-65 min;
preferably, the mixing in step S1 is ball milling mixing, the ball milling of the single-walled carbon nanotube and the aluminum matrix is performed for 25-35 min, the ball milling is stopped for 25-35 min, the circulation is performed for 2-4 times, and the ball milling mixing is performed for 115-125 min;
preferably, the pressure of the hot-pressing sintering in the step S2 is 5-10 MPa, and the sintering temperature is 520-580 ℃;
preferably, the hot press sintering of step S2 is performed in vacuum;
preferably, the multidirectional forging temperature in the step S3 is 250-350 ℃;
preferably, in the step S3, the forging pass of the multidirectional forging is 1-5 passes, the deformation of each pass is 25% -40%, and after the aluminum-based composite material blank is subjected to the multidirectional forging processing of multiple passes, the internal structure of the obtained composite material is further densified, which is beneficial to obtaining the composite material with uniform and fine structure and excellent performance.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the high-strength plastic single-walled carbon nanotube aluminum-based composite material, the strength of the composite material is improved by specially adding the single-walled carbon nanotubes (SCNTs) as a reinforcing phase; the preparation process generates a small amount of Al4C3The aluminum alloy also has the function of strengthening the aluminum matrix, and simultaneously, alloying elements Zn, Cu, Mg, Mn and Si in the aluminum matrix form second-phase solid solution strengthening or solid solution aluminum dispersion strengthening.
2. The high-strength plastic single-walled carbon nanotube aluminum-based composite material further improves the density and the strength through multidirectional forging, and the 6061 aluminum-based composite material has excellent comprehensive performance. Experimental tests show that the tensile strength of the aluminum-based composite material obtained by the invention is 220-320 MPa, and the elongation is 10-20%.
Drawings
FIG. 1 is a flow chart of the preparation method of the high-strength plastic single-wall carbon nanotube aluminum-based composite material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, so that those skilled in the art can fully understand the technical contents of the present invention. It should be noted that the specific embodiments described herein are only for explaining the present invention and are not used to limit the present invention.
The high-strength plastic single-walled carbon nanotube aluminum-based composite material takes 6061 aluminum alloy as an aluminum-based preparation composite material, and 0.05-0.4 w% of single-walled carbon nanotube (SCNT) with less reinforcing phase is addedt%, and 99.6-99.95 wt% of aluminum alloy as aluminum matrix phase 6061. Wherein 6061 aluminum alloy powder in the aluminum matrix is pre-alloy powder which is prepared according to the following components: 0.4-0.8 wt%; zn: less than or equal to 0.25 wt%; cu: 0.15-0.4 wt%; mg: 0.8-1.2 wt%; mn: less than or equal to 0.15 wt%; the balance being Al. The single-walled carbon nanotube is used as a reinforcing phase, and the strength of an aluminum matrix is effectively improved by the special preparation method. The preparation process generates a small amount of Al4C3The aluminum alloy also has the function of strengthening the aluminum matrix, and simultaneously, alloying elements Zn, Cu, Mg, Mn and Si in the aluminum matrix form second-phase solid solution strengthening or solid solution aluminum dispersion strengthening.
The invention also provides a preparation method of the high-strength plastic single-walled carbon nanotube aluminum-based composite material, the preparation method of the aluminum-based composite material adopts a powder metallurgy method and a multidirectional forging composite processing method, and the single-walled carbon nanotube/6061 aluminum-based composite material comprises the following steps:
a) mixing raw materials of 0.05 to 0.4 weight percent of enhanced phase single-walled carbon nanotube (SCNT) and 99.6 to 99.95 weight percent of aluminum matrix to obtain mixed powder; the aluminum matrix is pre-alloyed powder of 6061 aluminum alloy powder.
b) Carrying out vacuum hot-pressing sintering on the mixed powder obtained in the step a), wherein the sintering temperature is 520-580 ℃, and the pressure is 5-10 MPa;
c) and c) carrying out multidirectional forging and rolling composite technology on the aluminum matrix composite blank obtained in the step b) to obtain the high-performance aluminum matrix composite.
Step a) is a process of mixing raw materials, and in order to fully mix various raw materials, ball milling mixing ball milling is adopted for 30min, ball milling is stopped for 30min, ball milling is carried out for 120min, and 4 circulation times are preferred. The mixing mode of the invention mainly adopts vacuum dry grinding. Preferably, the single-walled carbon nanotube has a diameter of 1-20 nm and a length of 0.5-30 μm; the granularity of the 6061 prealloying powder is 5-50 microns, and as a preferable scheme, 0.1-0.2 wt% of dispersing agent is added into the prealloying powder raw material to enable the single-walled carbon nanotube to be uniformly dispersed in ultrasonic waves.
Step b) is the process of vacuum hot pressing sintering of the mixed powder, the sintering pressure is preferably 5MPa, and the pressing mode can be selected from the modes well known by the technical personnel in the field, such as placing the mixed powder in a graphite mold for bidirectional pressurization and placing the graphite mold into a sintering furnace, wherein the sintering temperature is 550 ℃, the pressure is 5MPa, and the heat preservation time is 1 hour.
The 6061 aluminum-based composite material obtained in the step c) is subjected to multidirectional forging and rolling, so that the internal structure of the aluminum-based composite material blank is further densified, and the composite material with uniform and fine structure and better performance can be obtained; the multidirectional forging temperature of (2) is preferably 350 ℃, and the number of passes is preferably 2. After the aluminum matrix composite material is sintered and is subjected to multidirectional forging, the strength and the elongation of the aluminum matrix composite material are further improved.
In the process of preparing the 6061 aluminum-based composite material, the high-performance 6061 aluminum-based composite material is obtained through a powder metallurgy sintering process and a multidirectional forging rolling process. In the powder sintering process, the single-walled carbon nanotubes are uniformly distributed in the 6061 aluminum alloy matrix, which is beneficial to improving the strength of the composite material, and the subsequent multidirectional forging process further strengthens the mechanical property of the aluminum-based composite material.
Example 1
(1) 0.05 wt% of single-walled carbon nanotube is subjected to ultrasonic dispersion for 1 hour, 0.15 wt% of Tween 80 dispersant is added, and aluminum alloy is 99.95 wt% of aluminum matrix, and the mixture is subjected to vacuum dry grinding for 120 minutes to obtain mixed powder; the pipe diameter of the single-walled carbon nanotube is 10-20 nanometers, and the length of the single-walled carbon nanotube is 20-30 micrometers; the grain size of the 6061 prealloyed powder is 35-50 microns,
(2) performing vacuum hot-pressing sintering on the mixed powder obtained in the step (1), wherein the sintering temperature is 550 ℃, and the pressure is 5MPa to obtain a blank;
(3) cutting the blank obtained in the step (2), and then performing multidirectional forging rolling processing, wherein the multidirectional forging is performed by performing 20% deformation in three directions respectively, and the forging temperature is 350 ℃;
the mechanical properties of the aluminum matrix composite prepared by the method are detected, and the results are shown in table 1.
Example 2
(1) The single-walled carbon nanotube accounts for 0.1 wt%, ultrasonic dispersion is carried out for 55min, 0.2 wt% of Tween 80 dispersant is added, and the matrix aluminum alloy accounts for 99.9 wt%. Carrying out vacuum dry grinding for 120 minutes to obtain mixed powder; the pipe diameter of the single-walled carbon nanotube is 1-10 nanometers, and the length of the single-walled carbon nanotube is 10-20 micrometers; the grain size of the 6061 prealloyed powder is 5-25 microns,
(2) performing vacuum hot-pressing sintering on the mixed powder obtained in the step (1) at the temperature of 520 ℃ and the pressure of 10MPa to obtain a blank;
(3) cutting the blank obtained in the step (2), and then performing multidirectional forging, wherein the three forging directions are respectively deformed by 30%, 29% and 25%, and the forging temperature is 300 ℃;
the performance of the aluminum matrix composite material prepared by the method is tested, and the results are shown in table 1.
Example 3
(1) 0.2 wt% of single-walled carbon nanotube, ultrasonic dispersion for 65min, and addition of 0.15 wt% of Tween 80 dispersant, wherein the matrix aluminum alloy accounts for 99.8 wt%. Carrying out vacuum dry grinding for 120 minutes to obtain mixed powder; the pipe diameter of the single-walled carbon nanotube is 1-20 nanometers, and the length of the single-walled carbon nanotube is 15-30 micrometers; the granularity of the 6061 prealloying powder is 15-30 microns;
(2) applying vacuum hot-pressing sintering temperature to the mixed powder obtained in the step (1) at 580 ℃, and applying pressure of 7.5MPa to obtain a blank;
(3) cutting the blank obtained in the step (2), and then performing multidirectional forging, wherein the blank is deformed in 31%, 27% and 27% in three directions respectively, and the forging temperature is 250 ℃;
the performance of the aluminum matrix composite material prepared by the method is tested, and the results are shown in table 1.
Example 4
(1) The single-walled carbon nanotube is ultrasonically dispersed for 65 minutes at the weight percent of 0.3 percent, and Tween 80 dispersant at the weight percent of 0.1 percent is added, and the matrix aluminum alloy is 99.7 percent. Carrying out vacuum dry grinding for 120 minutes to obtain mixed powder; the tube diameter of the single-walled carbon nanotube is 1-20 nanometers, and the length of the single-walled carbon nanotube is 0.5-30 micrometers; the grain size of the 6061 prealloyed powder is 5-50 microns,
(2) performing vacuum hot-pressing sintering on the mixed powder obtained in the step (1) at the temperature of 350 ℃ and under the pressure of 6MPa to obtain a blank;
(3) cutting the blank obtained in the step (2), and then performing multidirectional forging, wherein the three forging directions are respectively deformed by 40%, 38% and 35%, and the forging temperature is 280 ℃;
example 5
(1) The single-walled carbon nanotube is ultrasonically dispersed for 65 minutes at the weight percent of 0.4 percent, and Tween 80 dispersant at the weight percent of 0.1 percent is added, and the matrix aluminum alloy is 99.6 percent. Carrying out vacuum dry grinding for 120 minutes to obtain mixed powder; the tube diameter of the single-walled carbon nanotube is 1-20 nanometers, and the length of the single-walled carbon nanotube is 0.5-30 micrometers; the grain size of the 6061 prealloyed powder is 5-50 microns,
(2) performing vacuum hot-pressing sintering on the mixed powder obtained in the step (1) at the temperature of 550 ℃ and under the pressure of 8.5MPa to obtain a blank;
(3) cutting the blank obtained in the step (2), and then performing multidirectional forging, wherein the deformation in three directions of forging is respectively 30%, 35% and 40%, and the forging temperature is 320 ℃;
the performance of the aluminum matrix composite material prepared by the method is tested, and the results are shown in table 1.
Table 1 results of performance test of the aluminum matrix composite prepared in example
Group of Tensile strength (MPa) Elongation (%)
Example 1 216 18.4
Example 2 248 16.3
Example 3 272 12.4
Example 4 296 11.2
Example 5 315 10.5
As can be seen from Table 1, the aluminum matrix composite material provided by the invention has high comprehensive performance, can be subjected to performance combination by adjusting components and processing technology, and has wide application prospect. The high-strength plastic single-walled carbon nanotube aluminum-based composite material further improves the density and the strength through multidirectional forging, and the 6061 aluminum-based composite material has excellent comprehensive performance. Experimental tests show that the tensile strength of the aluminum-based composite material obtained by the invention is 220-320 MPa, and the elongation is 10-20%.
It should be noted that the above-mentioned preferred embodiments are merely illustrative of the technical concepts and features of the present invention, and are intended to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (10)

1. A high-strength plastic single-walled carbon nanotube aluminum-based composite material comprises 0.05 to 0.4 weight percent of single-walled carbon nanotube and 99.6 to 99.95 weight percent of aluminum matrix; wherein the aluminum matrix is pre-alloyed powder.
2. The high-strength plastic single-wall carbon nanotube aluminum-based composite material as claimed in claim 1, wherein: the pipe diameter of the single-walled carbon nanotube is 1-20 nanometers, and the length of the single-walled carbon nanotube is 0.5-30 micrometers; the grain size of the pre-alloyed powder is 5-50 microns.
3. A high strength plastic single wall carbon nanotube aluminum alloy based composite material as claimed in claim 1 or 2, wherein: the pre-alloyed powder comprises the following components: 0.4-0.8 wt%; zn: less than or equal to 0.25 wt%; cu: 0.15-0.4 wt%; mg: 0.8-1.2 wt%; mn: less than or equal to 0.15 wt%; the balance being Al.
4. The high-strength plastic single-wall carbon nanotube aluminum-based composite material as claimed in claim 3, wherein: 0.1-0.2 wt% of dispersing agent is also added into the pre-alloyed powder.
5. The preparation method of the high-strength plastic single-walled carbon nanotube aluminum-based composite material as claimed in any one of claims 1 to 4, comprising the following steps:
s1, mixing the raw materials, and respectively weighing the single-walled carbon nanotube and the aluminum matrix pre-alloy powder as the raw materials; dispersing and uniformly mixing the single-walled carbon nanotube and the aluminum matrix material in ultrasonic waves to obtain mixed powder;
s2, carrying out hot-pressing sintering on the powder uniformly mixed in the step S1 to obtain an aluminum-based composite material blank of 6061 aluminum alloy;
and S3, multi-directional forging, namely, carrying out multi-directional forging processing on the aluminum-based composite material blank obtained in the step S2 to obtain the high-strength plastic aluminum-based composite material.
6. The preparation method of the high-strength plastic single-wall carbon nanotube aluminum-based composite material as claimed in claim 5, wherein the preparation method comprises the following steps: the mixing is ball milling mixing, the ball milling of the single-walled carbon nanotube and the aluminum matrix is firstly carried out for 25-35 min, the ball milling is stopped for 25-35 min, the circulation is carried out for 2-4 times, and the ball milling mixing is carried out for 115-125 min.
7. The preparation method of the high-strength plastic single-wall carbon nanotube aluminum-based composite material as claimed in claim 5, wherein the preparation method comprises the following steps: and step S1, the ultrasonic dispersion time is 55-65 min.
8. The preparation method of the high-strength plastic single-wall carbon nanotube aluminum-based composite material as claimed in claim 5, wherein the preparation method comprises the following steps: and S2, performing hot-pressing sintering in vacuum, wherein the pressure of the hot-pressing sintering is 5-10 MPa, and the sintering temperature is 520-580 ℃.
9. The preparation method of the high-strength plastic single-wall carbon nanotube aluminum-based composite material as claimed in claim 5, wherein the preparation method comprises the following steps: in the step S3, the forging pass of the multidirectional forging is 1-5 passes, and the deformation of each pass is 25-40%.
10. The method for preparing the high-strength plastic single-wall carbon nanotube aluminum alloy matrix composite material as claimed in claim 9, is characterized in that: and step S3, wherein the multidirectional forging temperature is 250-350 ℃.
CN202110422450.XA 2021-04-20 2021-04-20 High-strength plastic single-walled carbon nanotube aluminum-based composite material and preparation method thereof Pending CN113136508A (en)

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