CN105734459A - Preparation method of carbon nanotube reinforced aluminum base composite material - Google Patents

Preparation method of carbon nanotube reinforced aluminum base composite material Download PDF

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Publication number
CN105734459A
CN105734459A CN201410767191.4A CN201410767191A CN105734459A CN 105734459 A CN105734459 A CN 105734459A CN 201410767191 A CN201410767191 A CN 201410767191A CN 105734459 A CN105734459 A CN 105734459A
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preparation
carbon nanotube
composite material
aluminium
powder
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CN105734459B (en
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陈名海
董占青
裴久阳
李清文
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Suzhou Institute of Nano Tech and Nano Bionics of CAS
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Abstract

The invention discloses a preparation method of a carbon nanotube reinforced aluminum base composite material. The preparation method comprises the following steps: a carbon nanotube, aluminum powder or aluminum ally powder and a process control agent are prepared to composite powder by ball milling; the composite powder is packed in a cover material, is heated to an appointed temperature for sintering, and is hotly extruded to prepare a composite material blank; and the cover material is stripped to obtain a target product. The preparation method adopts a thermal extrusion powder forming process, simplifies the technological flows of blank pressing, sintering and thermal extrusion molding in a traditional powder metallurgy process, realizes one-step molding, greatly improves the production efficiency, prevents the insulation time of a carbon nanotube and an aluminum matrix in a high-temperature area in a similar multi-step powder metallurgy process, prevents quick interface reaction of the carbon nanotube and the aluminum matrix, effectively controls effective interface bonding between the aluminum matrix and the carbon nanotube, is simple in preparation process, and broad in industrial application prospect, and effectively reduces the cost.

Description

The preparation method of carbon nanotube enhanced aluminium-based composite material
Technical field
Present invention relates particularly to the preparation method that a kind of CNT strengthens aluminum aluminum matrix composite, belong to the technical field of Nano-composite materials.
Background technology
Aluminum matrix composite has the advantages such as high-strength light, wear resistant corrosion resistant, heat-conductivity conducting and thermal coefficient of expansion are low, is widely used in the industry such as Aero-Space, automobile making, electronic machine, is also the Hot Contents of new material research both at home and abroad in the last few years.Meanwhile, CNT is as one-dimensional nano material, and tensile strength can reach 50 ~ 200GPa, it is approximately 100 times of steel, light weight, density is the 1/6 of steel, elastic modelling quantity is about 1TPa, and CNT has the electrical and thermal conductivity performance of excellence simultaneously, is considered optimal composite material reinforcement body.Carbon nanotube enhanced aluminium-based composite material, with its superior comprehensive mechanical property, is expected to become the high-strength light metal-base composites of new generation substituting traditional ceramics phase reinforced aluminum matrix composites.
Tradition carbon nanotube enhanced aluminium-based composite material preparation method include the methods such as powder metallurgic method, melting casting, Pressure Infiltration, electro-deposition, thermal spraying, wherein powder metallurgical technique due to its adaptation wide, be preparation method the most frequently used at present.But the problems such as the method ubiquity processing step that the current powder metallurgy adopted prepares carbon nanotube enhanced aluminium-based composite material is loaded down with trivial details, production efficiency is low.Such as, publication number be CN101956149A patent of invention in prepare carbon nano tube reinforced aluminum alloy composite material by ball-milled powder, technique compressing, vacuum-sintering, and assist secondary operations to improve the consistency of material further, reduce defect.The patent of invention that publication number is CN1834280A is prepared for carbon nano tube reinforced aluminum alloy composite material by vacuum hotpressing, it adopts high-energy ball milling 10-15 hour, the mental retardation ball milling two step-length time ball-milling methods of 20-25 hour, the subsequently operation such as compacting, sintering, whole flow process is longer.Publication number be CN102424919A patent of invention in by adopt ball milling, sintering, hot pressing, hot extrusion are prepared for carbon nanotube enhanced aluminium-based composite material.Therefore, explore high efficiency preparation method, to shorten flow process, reduce CNT and aluminum substrate and stop, in high-temperature region, the unfavorable interfacial reaction brought for a long time, it appears be particularly important.But position so far, still lacks a kind of not only effective but also economic method preparing carbon nanotube enhanced aluminium-based composite material.
Summary of the invention
Present invention is primarily targeted at the preparation method that a kind of carbon nanotube enhanced aluminium-based composite material is provided, it is simple that it has technique, production efficiency is high, and obtained carbon nanotube enhanced aluminium-based composite material has Good All-around Property, thus overcoming deficiency of the prior art.
For realizing aforementioned invention purpose, the technical solution used in the present invention includes:
A kind of preparation method of carbon nanotube enhanced aluminium-based composite material, including:
CNT, aluminium powder or Al alloy powder and process control agent are made composite granule through ball milling,
Described composite granule is packaged in sheath material, is heated to assigned temperature sintering, makes composite blank through hot extrusion,
And, peel off sheath material, it is thus achieved that target product.
Preferably, described composite granule comprises the following component calculated by weight: CNT 0.1-10 part, aluminium powder or Al alloy powder 90-99 part, process control agent 0.01-2 part.
Further, described CNT includes any one and the two or more combinations in SWCN, multi-walled carbon nano-tubes.
Comparatively preferred, the caliber of described CNT is 0.4 nanometer-150 nanometers.
Further, described aluminium powder or Al alloy powder are at least selected from pure aluminium powder, aluminum-silicon system, aluminum-magnesium series, Solder for Al-Cu Joint Welding system, aluminum-zinc system and rare earth aluminium alloy powder, but are not limited to this.
Comparatively preferred, the mean particle size of described aluminium powder or Al alloy powder is 50 nanometers-100 microns.
Further, described process control agent is at least selected from stearic acid, lithium stearate, zinc stearate, paraffin, methanol, ethanol, silicone oil, oleic acid, cellulose, but is not limited to this.
Comparatively preferred, the ball-milling technology condition adopted in this preparation method includes: ratio of grinding media to material is 1/1-40/1, and rotating speed is 100 revs/min-3500 revs/min, and Ball-milling Time is 30 minutes-6 hours.
Further, the ball-milling technology adopted in this preparation method is at least selected from planetary type ball-milling, stirring ball-milling technique, but is not limited to this.
Further, described sheath material can adopt metal capsule material, for instance be selected from but be not limited in copper, aluminum, iron pipe shape thin-wall section any one.
Comparatively preferred, the sintering temperature adopted in this preparation method is 400 DEG C-620 DEG C, and heat time heating time is 30 seconds-6 hours.
Comparatively preferred, the hot extrusion technique condition adopted in this preparation method includes: pressure is 10MPa-700MPa, and extrusion ratio is 4/1-50/1, extrusion speed is 2-10 mm/second.
Further, this preparation method may also include that after peeling off sheath material, removes the burr of composite blank, thus obtaining target product.
The present invention is by simplifying the technological process of blank compacting, sintering, heat extrusion forming in prior powder metallurgy technique, realize one-step shaping, substantially increase production efficiency, avoid CNT and the aluminum substrate temperature retention time in high-temperature region in similar multi-step powder metallurgical technique simultaneously, avoid the unfavorable interfacial reaction of CNT and aluminum substrate, effectively control the effective interface between aluminum substrate and CNT to combine, realize CNT being uniformly distributed in aluminium base, it is possible to prepare the carbon nanotube enhanced aluminium-based composite material with Good All-around Property.
Comparing to prior art, the present invention at least has the advantages that
(1) achieve the simplification to powder metallurgical technique, have the advantages that significant efficiency is high, energy consumption is low;
(2) avoid vacuum-sintering to heat up cooling and long-time high-temperature residence, be prevented effectively from high-temperature region deleterious interfacial reaction, it is thus achieved that high-quality composite;
(3) powder hot-roll forming is high temperature dynamic molding, is conducive to the densification of material.
Accompanying drawing explanation
Fig. 1 is a kind of carbon nanotube enhanced aluminium-based composite material preparation technology flow chart among the present invention one typical embodiments;
Fig. 2 is the mechanical property figure of the obtained carbon nanotube enhanced aluminium-based composite material of embodiment of the present invention 1-4;
Fig. 3 is the embodiment of the present invention 1 and the mechanical property figure of the obtained carbon nanotube enhanced aluminium-based composite material of 5-7;
Fig. 4 is the embodiment of the present invention 1 and the mechanical property figure of the obtained carbon nanotube enhanced aluminium-based composite material of 8-10.
Detailed description of the invention
Many defects in view of prior art, inventor is through studying for a long period of time and putting into practice in a large number, draw technical scheme, first CNT, aluminium powder or Al alloy powder, process control agent etc. are prepared composite granule through ball milling by it, and selecting process control agent is prevent CNT, aluminium powder or Al alloy powder from occurring cold welding phenomenon in mechanical milling process;Subsequently the composite granule obtained is encapsulated in metal capsule, reheats after being warming up to assigned temperature, prepare composite blank through hot extrusion, peel off sheath material subsequently, remove burr etc. and can obtain carbon nanotube enhanced aluminium-based composite material of good performance.
Below in conjunction with accompanying drawing and some embodiments, technical scheme is further described.
Embodiment 1Referring to Fig. 1, the preparation method of this carbon nanotube enhanced aluminium-based composite material includes:
Step one, successively by pure aluminium powder, process control agent stearic acid and mass percent that mean diameter is 20 microns be 1.5%, caliber be that the multi-walled carbon nano-tubes three of 40 nanometers mixes, adopt planetary type ball-milling technique, ratio of grinding media to material is 10/1, rotating speed 300 revs/min, Ball-milling Time 4 hours, prepares composite granule;
Step 2, being encapsulated in by prepared composite granule in copper pipe shape thin-walled material jacket, and preheat in electric furnace, sintering temperature 550 degree, heat time heating time is 2 hours;
Step 3, pressure are that 10MPa-700MPa, extrusion ratio 4/1-50/1, extrusion speed 2-10 mm/second are extruded.Hot extrusion removes jacket, burr after terminating, and finally obtains carbon nanotube enhanced aluminium-based composite material.Its organizational structure and mechanical performance data thereof are referring to Fig. 2-4.
Embodiment 2The present embodiment difference from embodiment 1 is in that, in step one, the percentage by weight of CNT is 0.5%.
Embodiment 3The present embodiment difference from embodiment 1 is in that, in step one, the percentage by weight of CNT is 1.0%.
Embodiment 4The present embodiment difference from embodiment 1 is in that, in step one, the percentage by weight of CNT is 2.0%.
Embodiment 5The present embodiment difference from embodiment 1 is in that, in step one, Ball-milling Time is 3h.
Embodiment 6The present embodiment difference from embodiment 1 is in that, in step one, Ball-milling Time is 5h.
Embodiment 7The present embodiment difference from embodiment 1 is in that, in step one, Ball-milling Time is 6h.
Embodiment 8The present embodiment difference from embodiment 1 is in that, in step 2, sintering temperature is 450 DEG C.
Embodiment 9The present embodiment difference from embodiment 1 is in that, in step 2, sintering temperature is 500 DEG C.
Embodiment 10The present embodiment difference from embodiment 1 is in that, in step 2, sintering temperature is 600 DEG C.
The mechanical property of carbon nanotube enhanced aluminium-based composite material, hardness data etc. obtained by embodiment 1-10 technique refer to Fig. 2-4.
Should be appreciated that described above, and in the embodiment shown on drawing, can not resolve is limited determines the design philosophy of the present invention.Holding identical skill in the technical field of the present invention can the technical thought of the present invention be changed with various form improvement, such improvement and change are interpreted as belonging in protection scope of the present invention.

Claims (11)

1. the preparation method of a carbon nanotube enhanced aluminium-based composite material, it is characterised in that including:
CNT 0.1-10%, aluminium powder or Al alloy powder 90-99% and process control agent 0.01-2% are made composite granule through ball milling, described composite granule is packaged in sheath material, it is heated to assigned temperature sintering, composite blank is made through hot extrusion, and, peel off sheath material, it is thus achieved that target product.
2. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterized in that described composite granule comprises the following component calculated by weight: CNT 0.1-10 part, aluminium powder or Al alloy powder 90-99 part, process control agent 0.01-2 part.
3. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1 and 2, it is characterized in that described CNT includes any one and two or more combinations in SWCN, multi-walled carbon nano-tubes, and the caliber of described CNT is 0.4 nanometer-150 nanometers.
4. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1 and 2, it is characterized in that described aluminium powder or Al alloy powder are at least selected from pure aluminium powder, aluminum-silicon system, aluminum-magnesium series, Solder for Al-Cu Joint Welding system, aluminum-zinc system and rare earth aluminium alloy powder, and the mean particle size of described aluminium powder or Al alloy powder is 50 nanometers-100 microns.
5. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1 and 2, it is characterised in that described process control agent is at least selected from stearic acid, lithium stearate, zinc stearate, paraffin, methanol, ethanol, silicone oil, oleic acid, cellulose.
6. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterized in that the ball-milling technology condition adopted in this preparation method includes: ratio of grinding media to material is 1/1-40/1, rotating speed is 100 revs/min-3500 revs/min, and Ball-milling Time is 30 minutes-6 hours.
7. the preparation method of the carbon nanotube enhanced aluminium-based composite material according to claim 1 or 6, it is characterised in that the ball-milling technology adopted in this preparation method is at least selected from planetary type ball-milling, stirring ball-milling technique.
8. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterised in that described sheath material adopts metal capsule material, and described metal capsule material includes any one in copper, aluminum, iron pipe shape thin-wall section.
9. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterised in that the sintering temperature adopted in this preparation method is 400 DEG C-620 DEG C, and heat time heating time is 30 seconds-6 hours.
10. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterized in that the hot extrusion technique condition adopted in this preparation method includes: pressure is 10MPa-700MPa, extrusion ratio is 4/1-50/1, extrusion speed is 2-10 mm/second.
11. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterised in that also include: after peeling off sheath material, remove the burr of composite blank, thus obtaining target product.
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Cited By (12)

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CN105112705A (en) * 2015-06-25 2015-12-02 中国航空工业集团公司北京航空材料研究院 Method for preparing graphene/aluminum composite material
CN106756166A (en) * 2016-12-01 2017-05-31 中国科学院金属研究所 A kind of preparation method of tough carbon nano-tube reinforced metal-matrix composite material high
CN107282929A (en) * 2017-07-11 2017-10-24 大连大学 Fiber alignment strengthens composite material by electric current direct heating powder hot extrusion preparation method and device
CN108504908A (en) * 2018-04-17 2018-09-07 福州大学 A kind of preparation method of carbon nanotube enhanced aluminium-based composite material
CN109182813A (en) * 2018-08-22 2019-01-11 天津大学 In the method for silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites
CN110331315A (en) * 2019-07-02 2019-10-15 南昌大学 A kind of method of carbon nanotube and the polynary reinforced aluminum matrix composites of compound rare-earth
CN111636006A (en) * 2020-05-29 2020-09-08 香港生产力促进局 Aluminum-silicon alloy graphite composite heat conduction material and preparation and application thereof
CN113427009A (en) * 2021-06-24 2021-09-24 西北工业大学 Composite material powder with reinforcement distributed in crystal and preparation and forming methods thereof
CN113462918A (en) * 2021-05-28 2021-10-01 西安理工大学 Preparation method of CNTs/Al-Li high-strength composite material
WO2021215575A1 (en) * 2020-04-22 2021-10-28 부경대학교 산학협력단 Method for manufacturing cooling pipe for electric vehicle powertrain, and cooling pipe manufactured thereby
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CN115415516A (en) * 2022-07-06 2022-12-02 湖南文昌新材科技股份有限公司 Carbon nano tube reinforced aluminum matrix composite precursor preparation device

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105112705A (en) * 2015-06-25 2015-12-02 中国航空工业集团公司北京航空材料研究院 Method for preparing graphene/aluminum composite material
CN106756166A (en) * 2016-12-01 2017-05-31 中国科学院金属研究所 A kind of preparation method of tough carbon nano-tube reinforced metal-matrix composite material high
CN107282929A (en) * 2017-07-11 2017-10-24 大连大学 Fiber alignment strengthens composite material by electric current direct heating powder hot extrusion preparation method and device
CN107282929B (en) * 2017-07-11 2019-05-07 大连大学 Fiber alignment enhances composite material by electric current direct heating powder hot extrusion preparation method and device
CN108504908A (en) * 2018-04-17 2018-09-07 福州大学 A kind of preparation method of carbon nanotube enhanced aluminium-based composite material
CN109182813A (en) * 2018-08-22 2019-01-11 天津大学 In the method for silicon micropowder surface in-situ growing carbon nano tube reinforced aluminum matrix composites
CN110331315A (en) * 2019-07-02 2019-10-15 南昌大学 A kind of method of carbon nanotube and the polynary reinforced aluminum matrix composites of compound rare-earth
WO2021215575A1 (en) * 2020-04-22 2021-10-28 부경대학교 산학협력단 Method for manufacturing cooling pipe for electric vehicle powertrain, and cooling pipe manufactured thereby
CN111636006A (en) * 2020-05-29 2020-09-08 香港生产力促进局 Aluminum-silicon alloy graphite composite heat conduction material and preparation and application thereof
CN111636006B (en) * 2020-05-29 2021-09-28 香港生产力促进局 Aluminum-silicon alloy graphite composite heat conduction material and preparation and application thereof
CN113462918B (en) * 2021-05-28 2022-04-26 西安理工大学 Preparation method of CNTs/Al-Li high-strength composite material
CN113462918A (en) * 2021-05-28 2021-10-01 西安理工大学 Preparation method of CNTs/Al-Li high-strength composite material
CN113427009A (en) * 2021-06-24 2021-09-24 西北工业大学 Composite material powder with reinforcement distributed in crystal and preparation and forming methods thereof
CN113427009B (en) * 2021-06-24 2022-08-30 西北工业大学 Composite material powder with reinforcement distributed in crystal and preparation and forming methods thereof
RU2780728C1 (en) * 2021-10-15 2022-09-29 федеральное государственное бюджетное образовательное учреждение высшего образования "Ульяновский государственный технический университет" Method for producing an aluminium-based nanostructural composite material
CN115415516A (en) * 2022-07-06 2022-12-02 湖南文昌新材科技股份有限公司 Carbon nano tube reinforced aluminum matrix composite precursor preparation device

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