CN105088111A - Preparation method of carbon nanotube reinforced aluminum matrix composite - Google Patents
Preparation method of carbon nanotube reinforced aluminum matrix composite Download PDFInfo
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Abstract
The invention provides a preparation method of a carbon nanotube reinforced aluminum matrix composite. The preparation method includes the steps that (1) carbon nanotubes are dispersed in an inertial organic solvent to obtain carbon nanotube dispersion liquid; (2) foamed aluminum is immersed in the carbon nanotube dispersion liquid obtained the step (1), and the carbon nanotubes are dispersed in the foamed aluminum; (3) the foamed aluminum, containing the carbon nanotubes, in the step (2) are dried to obtain a carbon nanotube-foamed aluminum compound; and (4) the carbon nanotube-foamed aluminum compound obtained in the step (3) is subjected to hot pressing sintering, and then the carbon nanotube reinforced aluminum matrix composite is obtained after mold hot extrusion molding. Damage caused by a traditional ball-milling process to the carbon nanotubes is avoided, the performance of original carbon nanotubes is reserved, and process steps are also greatly simplified. The preparation method is low in cost, convenient to operate, short in preparation period and suitable for industrial volume production, and has high practicality.
Description
Technical field
The invention belongs to metal composite field, specifically refer to a kind of preparation method of carbon nanotube enhanced aluminium-based composite material.
Background technology
Metal-base composites has the premium properties of traditional metal materials, can overcome the performance limitation of traditional metal materials after adding wild phase.The advantages such as aluminum matrix composite has quality light, and intensity is high, wear resistant corrosion resistant, and the good and thermal expansivity of electrical and thermal conductivity is low, are widely used in space flight and aviation, automobile making, the industrial circles such as electronic machine.How carbon nanotube, as the common wild phase of one of aluminum matrix composite, utilizes the high performance aluminum matrix composite of carbon nanotube to become the focus studied this year both at home and abroad.
The dispersiveness of carbon nanotube in aluminum substrate is one of important factor affecting composite property.Traditional technology is being prepared in carbon nanotube enhanced aluminium-based composite material process, and the general method adopting ball milling, although can make the dispersion that carbon nanotube is good in aluminum substrate, causes damage to carbon nanotube to a certain extent, affect the performance of matrix material.How to prepare favorable dispersity, and carbon nanotube structure can be allowed complete is the subject matter needing at present to solve with the aluminum matrix composite making full use of carbon nanotube premium properties.
Summary of the invention
The object of the invention is the preparation method providing a kind of carbon nanotube enhanced aluminium-based composite material according to above-mentioned deficiency, the method technique is simple, is beneficial to mass production, and obtained Properties of Aluminum Matrix Composites is outstanding.
The present invention is achieved in the following ways: a kind of preparation method of carbon nanotube enhanced aluminium-based composite material, and its step comprises:
(1) carbon nanotube dispersed is obtained in inert organic solvents the carbon nano tube dispersion liquid that mass concentration is 0.1-10%;
(2) foamed aluminium is immersed in the carbon nano tube dispersion liquid described in step (1), makes carbon nanotube dispersed in foamed aluminium;
(3) carbon nanotube-foamed aluminium complex body is obtained step (2) Suo Shu containing after the foamed aluminium drying of carbon nanotube;
(4) by described for step (3) carbon nanotube-foamed aluminium complex body hot pressed sintering, then after mold hot extrusion forming, described carbon nanotube enhanced aluminium-based composite material is obtained.
Preferably, in described step (1), inert organic solvents is at least one in ethanol, ethylene glycol, glycerol, Virahol, butanols, acetone, butanone, hexanaphthene, heptane, ethyl acetate, toluene, dimethylbenzene, N methyl-2-pyrrolidone.
Preferably, described step also adds dispersion agent in (1), the weight ratio of described dispersion agent and carbon nanotube is 0.1-5:1, and described dispersion agent is at least one in Mierocrystalline cellulose, methylcellulose gum, Walocel MT 20.000PV, polyacrylic acid, Polyvinylpyrolidone (PVP), polysorbate, polyoxyethylene glycol, polypropylene glycol, alkylolamide.Preferably, first by carbon nanotube and dispersant, then adopt ball milling, ultrasonic, grinding or the dispersing mode of high speed shear by carbon nanotube dispersed in inert organic solvents.
Preferably, the carbon nanotube diameter in described step (1) is 0.4-150nm, and length is 200nm-1mm.
Preferably, the foamed aluminium of described step (2) is the foamed aluminium that the first zone of oxidation washing away top layer in an acidic solution carries out overactivation process.Described acidic solution can be any one of hydrochloric acid, acetic acid, nitric acid, sulfuric acid or phosphoric acid.
Preferably, the drying in described step (3) is the oven dry carried out at 100-200 DEG C.
Preferably, the hot pressed sintering in described step (4), temperature is 450-620 DEG C, and pressure is 10-1000MPa, and the hot pressed sintering time is 0.5-2 hour.
Preferably, the heat extrusion forming in described step (4), extrusion ratio is 4-25:1, extrusion temperature 450-620 DEG C, squeeze pressure 100-1000Mpa.
Preferably, in described carbon nanotube enhanced aluminium-based composite material, the weight of carbon nanotube accounts for the 0.5-5% of foamed aluminium weight.
Carbon nanotube is first uniformly dispersed by the present invention in organic solvent, is conducive to carbon nanotube and is uniformly distributed in foamed aluminium.Then utilize the communicating aperture of foamed aluminium, make carbon nano tube dispersion liquid pass through to enter in foamed aluminium communicating aperture and can be dispersed in foamed aluminium.Because foamed aluminium communicating aperture is relatively more even, therefore carbon nanotube dispersed is also very even in foamed aluminium.Meanwhile, preparation method of the present invention avoids the destruction that traditional ball-milling technology causes carbon nanotube, remains the performance of original carbon nanotube, but also enormously simplify processing step.In addition, the process of hot pressed sintering ensure that the densification of material, by controlling hot compression parameters in its process, can realize the regulation and control to microstructure of composite structure and interfacial characteristics.Finally prepare described carbon nanotube enhanced aluminium-based composite material by large plastometric set hot extrude again, the performance of the aluminum matrix composite of gained is improved.Preparation method's cost of the present invention is lower, easy to operate, preparation cycle is shorter, is applicable to industrialized mass production, has very strong practicality.
Embodiment
Embodiment 1
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 1.0g carbon nanotube, (diameter of carbon nanotube is 10nm, length is 200nm, thered is provided by Chengdu is organic) and 2g dispersion agent Mierocrystalline cellulose mixing, then be added in 97g ethanol, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 1.0wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 100 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 580 DEG C, under pressure is 700MPa, carries out hot pressed sintering 1h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 580 DEG C, under 700MPa, carry out hot extrude with the hot extrude of 25:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 1.In described carbon nanotube enhanced aluminium-based composite material 1, the weight of carbon nanotube accounts for 1% of foamed aluminium weight.
Embodiment 2
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 2.0g carbon nanotube, (diameter of carbon nanotube is 10nm, length is 500nm) and 0.8g dispersion agent polyoxyethylene glycol mixing, then be added in 97.2g acetone, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 2.0wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 150 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 580 DEG C, under pressure is 700MPa, carries out hot pressed sintering 2h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 580 DEG C, under 700MPa, carry out hot extrude with the hot extrude of 25:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 2.In described carbon nanotube enhanced aluminium-based composite material 2, the weight of carbon nanotube accounts for 1.5% of foamed aluminium weight.
Embodiment 3
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 3.0g carbon nanotube, (diameter of carbon nanotube is 100nm, length is 1mm) and 0.8g dispersion agent polysorbate mixing, then be added in 96.2g hexanaphthene, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 3.0wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 200 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 450 DEG C, under pressure is 1000MPa, carries out hot pressed sintering 1h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 650 DEG C, under 1000MPa, carry out hot extrude with the hot extrude of 25:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 3.In described carbon nanotube enhanced aluminium-based composite material 3, the weight of carbon nanotube accounts for 2% of foamed aluminium weight.
Embodiment 4
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 4.0g carbon nanotube, (diameter of carbon nanotube is 150nm, length is 500nm) and 0.8g polyethylene of dispersing agent base pyrrolidone mixing, then be added in 95.2g toluene, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 3.0wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 100 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 620 DEG C, under pressure is 100MPa, carries out hot pressed sintering 1h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 450 DEG C, under 100MPa, carry out hot extrude with the hot extrude of 25:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 4.In described carbon nanotube enhanced aluminium-based composite material 4, the weight of carbon nanotube accounts for 2.5% of foamed aluminium weight.
Embodiment 5
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 5.0g carbon nanotube, (diameter of carbon nanotube is 0.4nm, length is 200nm) and 0.8g dispersion agent polyacrylic acid mixing, then be added in 94.2g ethyl acetate, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 3.0wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 100 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 600 DEG C, under pressure is 900MPa, carries out hot pressed sintering 0.5h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 600 DEG C, under 900MPa, carry out hot extrude with the hot extrude of 25:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 5.In described carbon nanotube enhanced aluminium-based composite material 5, the weight of carbon nanotube accounts for 3% of foamed aluminium weight.
Embodiment 6
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 6.0g carbon nanotube, (diameter of carbon nanotube is 10nm, length is 500nm) and 0.8g dispersion agent alkylolamide mixing, then be added in 93.2g dimethylbenzene, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 6.0wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 100 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 600 DEG C, under pressure is 900MPa, carries out hot pressed sintering 1h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 600 DEG C, under 900MPa, carry out hot extrude with the hot extrude of 16:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 6.In described carbon nanotube enhanced aluminium-based composite material 6, the weight of carbon nanotube accounts for 3.5% of foamed aluminium weight.
Embodiment 7
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 0.1g carbon nanotube, (diameter of carbon nanotube is 10nm, length is 500nm) and the dispersion agent methylcellulose gum of 0.5g mix with Walocel MT 20.000PV, then be added in 99.4g Virahol and alcohol mixed solvent, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 0.1wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 100 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 600 DEG C, under pressure is 900MPa, carries out hot pressed sintering 1h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 600 DEG C, under 900MPa, carry out hot extrude with the hot extrude of 4:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 7.In described carbon nanotube enhanced aluminium-based composite material 7, the weight of carbon nanotube accounts for 0.5% of foamed aluminium weight.
Embodiment 8
A preparation method for carbon nanotube enhanced aluminium-based composite material, specifically comprises the following steps:
(1) by 10.0g carbon nanotube, (diameter of carbon nanotube is 10nm, length is 500nm) and 1g dispersion agent polypropylene glycol mixing, then be added in 89gN-methyl-2-pyrrolidone, utilize ultrasonic disperse 1 hour, obtain carbon nano tube dispersion liquid (carbon nanotube is 10.0wt% at carbon nano tube dispersion liquid content).
(2) 20g communicating aperture foamed aluminium is placed on cleaning in the dilute hydrochloric acid of 5.0wt% and removes zone of oxidation post-drying.Communicating aperture foamed aluminium after activation treatment is immersed in carbon nano tube dispersion liquid, soaks after 2 hours and take out.
(3) dried in vacuum drying oven by the foamed aluminium containing carbon nanotube and obtain carbon nanotube-foamed aluminium complex body, in vacuum drying oven, vacuum tightness is 0.05mbar, and bake out temperature is 100 degree.
(4) carbon nanotube-foamed aluminium complex body is placed in electric furnace and is preheated to 600 DEG C, under pressure is 900MPa, carries out hot pressed sintering 1h.Then by the carbon nanotube after hot pressed sintering-foamed aluminium complex body 600 DEG C, under 900MPa, carry out hot extrude with the hot extrude of 16:1 ratio, obtain described carbon nanotube enhanced aluminium-based composite material 8.In described carbon nanotube enhanced aluminium-based composite material 8, the weight of carbon nanotube accounts for 5% of foamed aluminium weight.
Obtained by embodiment 1-8 carbon nanotube enhanced aluminium-based composite material 1-8 tensile strength of mechanical property and hardness as shown in table 1:
| Tensile strength Mpa | Hardness HBW | |
| Embodiment 1 | 173±8 | 66±3 |
| Embodiment 2 | 181±10 | 72±4 |
| Embodiment 3 | 212±6 | 84±3 |
| Embodiment 4 | 228±8 | 89±3 |
| Embodiment 5 | 282±6 | 103±2 |
| Embodiment 6 | 271±7 | 93±4 |
| Embodiment 7 | 160±5 | 68±3 |
| Embodiment 8 | 240±6 | 86±3 |
Table 1 carbon nanotube enhanced aluminium-based composite material 1-8 tensile strength and hardness
As can be seen from Table 1, the carbon nanotube enhanced aluminium-based composite material prepared by the inventive method can the tensile strength of reinforced aluminum matrix composites and hardness.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a preparation method for carbon nanotube enhanced aluminium-based composite material, its step comprises:
(1) carbon nanotube dispersed is obtained in inert organic solvents the carbon nano tube dispersion liquid that mass concentration is 0.1-10%;
(2) foamed aluminium is immersed in the carbon nano tube dispersion liquid described in step (1), makes carbon nanotube dispersed in foamed aluminium;
(3) carbon nanotube-foamed aluminium complex body is obtained step (2) Suo Shu containing after the foamed aluminium drying of carbon nanotube;
(4) by described for step (3) carbon nanotube-foamed aluminium complex body hot pressed sintering, then after mold hot extrusion forming, described carbon nanotube enhanced aluminium-based composite material is obtained.
2. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, is characterized in that: in described step (1), inert organic solvents is at least one in ethanol, ethylene glycol, glycerol, Virahol, butanols, acetone, butanone, hexanaphthene, heptane, ethyl acetate, toluene, dimethylbenzene, N-Methyl pyrrolidone.
3. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterized in that: described step also adds dispersion agent in (1), the weight ratio of described dispersion agent and carbon nanotube is 0.1-5:1, and described dispersion agent is at least one in Mierocrystalline cellulose, methylcellulose gum, Walocel MT 20.000PV, polyacrylic acid, Polyvinylpyrolidone (PVP), polysorbate, polyoxyethylene glycol, polypropylene glycol, alkylolamide.
4. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterized in that: the carbon nanotube diameter in described step (1) is 0.4-150nm, length is 200nm-1mm.
5. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, is characterized in that: the foamed aluminium of described step (2) is the foamed aluminium that the zone of oxidation first washing away top layer in an acidic solution carries out overactivation process.
6. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, is characterized in that: the drying in described step (3) is the oven dry carried out at 100-200 DEG C.
7. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterized in that: the hot pressed sintering in described step (4), temperature is 450-620 DEG C, and pressure is 100-1000MPa, and the hot pressed sintering time is 0.5-2 hour.
8. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterized in that: the heat extrusion forming in described step (4), extrusion ratio is 4-25:1, and extrusion temperature is 450-620 DEG C, and squeeze pressure is 100-1000Mpa.
9. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, is characterized in that: in described carbon nanotube enhanced aluminium-based composite material, the weight of carbon nanotube accounts for the 0.5-5% of foamed aluminium weight.
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| CN109321775A (en) * | 2018-11-12 | 2019-02-12 | 北京科技大学 | A method of preparing the Cu-base composites of carbon nano-tube oriented alignment |
| CN109913776A (en) * | 2019-03-28 | 2019-06-21 | 中国飞机强度研究所 | A kind of fiber reinforcement Open-cell Aluminum Foam and preparation method thereof |
| CN110611029A (en) * | 2019-09-04 | 2019-12-24 | 北京华碳元芯电子科技有限责任公司 | Method for preparing carbon nano tube film by printing method |
| CN113462918A (en) * | 2021-05-28 | 2021-10-01 | 西安理工大学 | Preparation method of CNTs/Al-Li high-strength composite material |
| CN115821104A (en) * | 2022-11-30 | 2023-03-21 | 国网浙江省电力有限公司湖州供电公司 | Method for preparing carbon nano tube modified aluminum-based composite material by adopting foamed aluminum adsorption |
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| CN113462918A (en) * | 2021-05-28 | 2021-10-01 | 西安理工大学 | Preparation method of CNTs/Al-Li high-strength composite material |
| CN113462918B (en) * | 2021-05-28 | 2022-04-26 | 西安理工大学 | Preparation method of CNTs/Al-Li high-strength composite material |
| CN115821104A (en) * | 2022-11-30 | 2023-03-21 | 国网浙江省电力有限公司湖州供电公司 | Method for preparing carbon nano tube modified aluminum-based composite material by adopting foamed aluminum adsorption |
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