CN105734459B - The preparation method of carbon nanotube enhanced aluminium-based composite material - Google Patents
The preparation method of carbon nanotube enhanced aluminium-based composite material Download PDFInfo
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- CN105734459B CN105734459B CN201410767191.4A CN201410767191A CN105734459B CN 105734459 B CN105734459 B CN 105734459B CN 201410767191 A CN201410767191 A CN 201410767191A CN 105734459 B CN105734459 B CN 105734459B
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Abstract
The invention discloses a kind of preparation method of carbon nanotube enhanced aluminium-based composite material, it includes：Composite granule is made by ball milling in CNT, aluminium powder or Al alloy powder and process control agent；The composite granule is packaged in sheath material, assigned temperature sintering is heated to, composite blank is pressed into through hot extrusion；And, sheath material is peeled off, target product is obtained.The present invention uses powder hot extrusion molding technique, simplifies blank compacting in prior powder metallurgy technique, sintering, the technological process of heat extrusion forming, realizes one-step shaping, substantially increases production efficiency；The soaking time of CNT and aluminum substrate in high-temperature region in similar multi-step powder metallurgical technique is avoided simultaneously, it is to avoid the quick interface reaction of CNT and aluminum substrate, the effective interface effectively controlled between aluminum substrate and CNT is combined；And preparation technology is simple, cost is effectively reduced, with wide industrial applications prospect.
Description
Technical field
Present invention relates particularly to the preparation method that a kind of CNT strengthens aluminium aluminum matrix composite, belong to nano combined material
Expect the technical field prepared.
Background technology
Aluminum matrix composite has high-strength light, wear resistant corrosion resistant, thermal conductivity and the low advantage of thermal coefficient of expansion, extensively
It is general to be applied to the industry such as Aero-Space, automobile making, electronic instrument, it is also in the last few years in the focus of domestic and international new material research
Hold.Meanwhile, CNT can reach 50 ~ 200 GPa as one-dimensional nano material, tensile strength, be approximately 100 times of steel,
Light weight, density is the 1/6 of steel, and modulus of elasticity is about 1 TPa, while CNT has excellent electrical and thermal conductivity performance, quilt
It is considered as optimal composite material reinforcement body.Carbon nanotube enhanced aluminium-based composite material has with its superior comprehensive mechanical property
Hoping turns into the high-strength light metal-base composites of new generation for substituting traditional ceramics phase reinforced aluminum matrix composites.
The preparation method of traditional carbon nanotube enhanced aluminium-based composite material includes powder metallurgic method, melting casting, pressure leaching
Ooze, electro-deposition, the method such as thermal spraying, wherein powder metallurgical technique due to its adaptation it is wide, be preparation method the most frequently used at present.
But the method generally existing processing step that the powder metallurgy used at present prepares carbon nanotube enhanced aluminium-based composite material is cumbersome, raw
Produce the low problem of efficiency.For example, by ball-milled powder, compressing, true in Publication No. CN101956149A patent of invention
The technique of sky sintering prepares carbon nano tube reinforced aluminum alloy composite material, and aids in secondary operation further to improve material
Consistency, reduces defect.Publication No. CN1834280A patent of invention is prepared for CNT by vacuum hotpressing strengthens aluminium
Alloy composite materials, it uses high-energy ball milling 10-15 hours, the low energy ball milling two step-length time ball-milling methods of 20-25 hours, then
The processes such as compacting, sintering, whole flow process is longer.In Publication No. CN102424919A patent of invention by using by ball milling,
Sintering, hot pressing, hot extrusion are prepared for carbon nanotube enhanced aluminium-based composite material.Therefore, high efficiency preparation method is explored, to shorten stream
Journey, reduces long-time of the CNT with aluminum substrate in high-temperature region and stops the unfavorable interfacial reaction brought, it appears be particularly important.But
Position, still lacks a kind of not only effective but also economic method for preparing carbon nanotube enhanced aluminium-based composite material so far.
The content of the invention
It is a primary object of the present invention to provide a kind of preparation method of carbon nanotube enhanced aluminium-based composite material, it has
Technique is simple, and production efficiency is high, and obtained carbon nanotube enhanced aluminium-based composite material has Good All-around Property, so as to overcome
Deficiency of the prior art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
A kind of preparation method of carbon nanotube enhanced aluminium-based composite material, including：
Composite granule is made by ball milling in CNT, aluminium powder or Al alloy powder and process control agent,
The composite granule is packaged in sheath material, assigned temperature sintering is heated to, is pressed into through hot extrusion multiple
Condensation material blank,
And, sheath material is peeled off, target product is obtained.
It is preferred that, the composite granule includes the following component calculated by weight：0.1-10 parts of CNT, aluminium powder or
90-99 parts of Al alloy powder, 0.01-2 parts of process control agent.
Further, the CNT includes any one in single-walled carbon nanotube, multi-walled carbon nanotube and two kinds
Combination above.
More preferred, the caliber of the CNT is 0.4 nanometer -150 nanometers.
Further, the aluminium powder or Al alloy powder at least may be selected from pure aluminium powder, aluminium-silicon systems, aluminum-magnesium series, Solder for Al-Cu Joint Welding system,
Aluminium-zinc system and rare earth aluminium alloy powder, but not limited to this.
More preferred, the mean particle size of the aluminium powder or Al alloy powder is 50 nanometers -100 microns.
Further, the process control agent at least may be selected from stearic acid, lithium stearate, zinc stearate, paraffin, methanol,
Ethanol, silicone oil, oleic acid, cellulose, but not limited to this.
More preferred, the ball-milling technology condition used in the preparation method includes：Ratio of grinding media to material is 1/1-40/1, and rotating speed is
100 revs/min -3500 revs/min, Ball-milling Time is -6 hours 30 minutes.
Further, the ball-milling technology used in the preparation method at least may be selected from planetary type ball-milling, stirring ball-milling technique,
But not limited to this.
Further, the sheath material can use metal capsule material, for example, may be selected from but be not limited to copper, aluminium, iron pipe
Any one in shape thin-wall section.
More preferred, the sintering temperature used in the preparation method is 400 DEG C -620 DEG C, and the heat time is 30 seconds -6 small
When.
More preferred, the hot extrusion technique condition used in the preparation method includes：Pressure is 10MPa-700MPa, is squeezed
Pressure ratio is that 4/1-50/1, extrusion speed are 2-10 mm/seconds.
Further, the preparation method may also include：After sheath material is peeled off, the flash of composite blank is removed,
So as to obtain target product.
The present invention is suppressed by simplifying blank in prior powder metallurgy technique, the technological process of sintering, heat extrusion forming, is realized
One-step shaping, substantially increases production efficiency, while avoiding CNT and aluminium base in similar multi-step powder metallurgical technique
Soaking time of the body in high-temperature region, it is to avoid the unfavorable interfacial reaction of CNT and aluminum substrate, effectively controls aluminum substrate and carbon
Effective interface between nanotube is combined, and is realized CNT being uniformly distributed in aluminium base, can be prepared with excellent comprehensive
Close the carbon nanotube enhanced aluminium-based composite material of performance.
Compared to prior art, the present invention at least has the advantages that：
（1）Realize the simplification to powder metallurgical technique, with significant efficiency high, energy consumption is low the characteristics of；
（2）Vacuum-sintering heating cooling and long-time high-temperature residence are avoided, deleterious interfacial in high-temperature region is prevented effectively from and reacts,
Obtain high-quality composite；
（3）Powder hot-roll forming is high temperature dynamic molding, is conducive to the densification of material.
Brief description of the drawings
Fig. 1 is a kind of carbon nanotube enhanced aluminium-based composite material preparation technology flow among a typical embodiments of the invention
Figure；
Fig. 2 is the mechanical property figure that 1-4 of the embodiment of the present invention obtains carbon nanotube enhanced aluminium-based composite material；
Fig. 3 is the mechanical property figure that the embodiment of the present invention 1 and 5-7 obtain carbon nanotube enhanced aluminium-based composite material；
Fig. 4 is the mechanical property figure that the embodiment of the present invention 1 and 8-10 obtain carbon nanotube enhanced aluminium-based composite material.
Embodiment
In view of many defects of prior art, inventor has drawn the present invention's through studying for a long period of time and largely putting into practice
Technical scheme, CNT, aluminium powder or Al alloy powder, process control agent etc. are prepared composite powder by it by ball milling first
Body, is to prevent CNT, aluminium powder or Al alloy powder from occurring cold welding phenomenon in mechanical milling process from process control agent；Then will
Obtained composite granule is encapsulated in metal capsule, and reheating is warming up to after assigned temperature, and composite wood is prepared through hot extrusion
Material base material, then peels off sheath material, goes Burr removal etc. to obtain carbon nanotube enhanced aluminium-based composite material of good performance.
Technical scheme is further described below in conjunction with accompanying drawing and some embodiments.
Embodiment 1 includes referring to Fig. 1, the preparation method of the carbon nanotube enhanced aluminium-based composite material：
Step 1: being by the pure aluminium powder that average grain diameter is 20 microns, process control agent stearic acid and mass percent successively
1.5%th, caliber is mixed for 40 nanometers of multi-walled carbon nanotube three, and using planetary type ball-milling technique, ratio of grinding media to material is 10/1,
Composite granule is made in 300 revs/min of rotating speed, Ball-milling Time 4 hours；
Step 2: obtained composite granule is encapsulated in copper pipe shape thin-walled material jacket, and preheated in electric furnace,
550 degree of sintering temperature, the heat time is 2 hours；
Step 3: pressure is 10MPa-700MPa, extrusion ratio 4/1-50/1, extrusion speed 2-10 mm/second extrusion formings.
Hot extrusion removes jacket, flash after terminating, and finally obtains carbon nanotube enhanced aluminium-based composite material.Its institutional framework and its mechanics
Performance data is referring to Fig. 2-4.
The present embodiment of embodiment 2 and the difference of embodiment 1 are that the percentage by weight of CNT is in step one
0.5%。
The present embodiment of embodiment 3 and the difference of embodiment 1 are that the percentage by weight of CNT is in step one
1.0%。
The present embodiment of embodiment 4 and the difference of embodiment 1 are that the percentage by weight of CNT is in step one
2.0%。
The present embodiment of embodiment 5 and the difference of embodiment 1 are that Ball-milling Time is 3 h in step one.
The present embodiment of embodiment 6 and the difference of embodiment 1 are that Ball-milling Time is 5 h in step one.
The present embodiment of embodiment 7 and the difference of embodiment 1 are that Ball-milling Time is 6 h in step one.
The present embodiment of embodiment 8 and the difference of embodiment 1 are that sintering temperature is 450 DEG C in step 2.
The present embodiment of embodiment 9 and the difference of embodiment 1 are that sintering temperature is 500 DEG C in step 2.
The present embodiment of embodiment 10 and the difference of embodiment 1 are that sintering temperature is 600 DEG C in step 2.
Mechanical property, hardness data of carbon nanotube enhanced aluminium-based composite material etc. please as obtained by embodiment 1-10 techniques
Refering to Fig. 2-4.
It should be appreciated that it is described above, and in the embodiment shown on drawing, the fixed design of the invention that is limited can not be parsed and thought
Think.Holding identical skill in the technical field of the present invention can be improved the technical thought of the present invention with various form
Change, such improvement and change are interpreted as belonging in protection scope of the present invention.
Claims (7)
1. a kind of preparation method of 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 passed through into ball milling system
Into composite granule, wherein, the process control agent is at least selected from stearic acid, lithium stearate, zinc stearate, paraffin, methanol, second
Alcohol, silicone oil, oleic acid, cellulose, the ball-milling technology condition include：Ratio of grinding media to material is 1/1-40/1, rotating speed is 100 revs/min-
3500 revs/min, Ball-milling Time is -6 hours 30 minutes；
The composite granule is packaged in sheath material, assigned temperature sintering is heated to, composite wood is pressed into through hot extrusion
Material base material, and, sheath material is peeled off, target product is obtained；
Wherein, the sintering temperature is 400 DEG C -620 DEG C, and the heat time is -6 hours 30 seconds；The hot extrusion technique condition bag
Include：Pressure is 10MPa-700MPa, and extrusion ratio is that 4/1-50/1, extrusion speed are 2-10 mm/seconds.
2. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterised in that described multiple
Close powder and include the following component calculated by weight：90-99 parts of 0.1-10 parts of CNT, aluminium powder or Al alloy powder, process
0.01-2 parts of controlling agent.
3. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1 or 2, it is characterised in that described
CNT includes any one and two or more combinations in single-walled carbon nanotube, multi-walled carbon nanotube, and the carbon is received
The caliber of mitron is 0.4 nanometer -150 nanometers.
4. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1 or 2, it is characterised in that described
Aluminium powder or Al alloy powder are at least selected from pure aluminium powder, aluminium-silicon systems, aluminum-magnesium series, Solder for Al-Cu Joint Welding system, aluminium-zinc system and rare earth aluminium alloy powder, and
The mean particle size of the 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, it is characterised in that the preparation
The ball-milling technology used in method is at least selected from planetary type ball-milling, stirring ball-milling technique.
6. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterised in that the bag
Cover material uses metal capsule material, and the metal capsule material includes any one in copper, aluminium, iron pipe shape thin-wall section.
7. the preparation method of carbon nanotube enhanced aluminium-based composite material according to claim 1, it is characterised in that also include：
After sheath material is peeled off, the flash of composite blank is removed, so as to obtain target product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| 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 |
| KR102298678B1 (en) * | 2020-04-22 | 2021-09-07 | 부경대학교 산학협력단 | Method for manufacturing cooling pipe for electric vehicle powertrain and cooling pipe manufactured thereby |
| 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 |
| 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 |
| 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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