CN103757569B - Ordered carbon nanotube reinforced aluminum matrix composites and preparation method thereof - Google Patents
Ordered carbon nanotube reinforced aluminum matrix composites and preparation method thereof Download PDFInfo
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- CN103757569B CN103757569B CN201310428335.9A CN201310428335A CN103757569B CN 103757569 B CN103757569 B CN 103757569B CN 201310428335 A CN201310428335 A CN 201310428335A CN 103757569 B CN103757569 B CN 103757569B
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Abstract
The invention discloses a kind of ordered carbon nanotube reinforced aluminum matrix composites and preparation method thereof.This matrix material comprises as the aluminium of body material or its alloy and the carbon nanotube that is scattered in order in described body material.The method comprises: plural ordered carbon nanotube thin film layer and plural aluminium or the cross layered rear hot rolling of its alloy layer are formed described ordered carbon nanotube reinforced aluminum matrix composites; Described ordered carbon nanotube thin film layer is formed by the plural carbon nanotube of ordered distribution.The present invention adopts ordered carbon nanotube film, such as, after super in-line arrangement carbon nano-tube films etc. and aluminium foil lamination, hot rolling is for matrix material, realize the distribution of orientations of carbon nanotube in aluminum substrate, give full play to mechanical property and the functional performance of carbon nanotube self excellence, realize to aluminum matrix composite mechanics strengthen and function modified, shaping in conjunction with hot rolling technique, there is important actual application prospect.
Description
Technical field
The present invention relates to a kind of preparation technology of aluminum matrix composite, be related specifically to a kind of ordered carbon nanotube reinforced aluminum matrix composites and preparation method thereof.
Background technology
Structure lightened is aerospace, communications and transportation, the great demand of power transmission and industrial equipment and development trend, is energy-saving and emission-reduction, the key issue that improves efficiency, increase voyage load, reduce working cost.Wherein lightweight structure material is key core technology, for hard-core technology and Important Project provide critical support material.As Novel light metal-base composites, carbon nanotube enhanced aluminium-based composite material is with its lightweight, high-strength, high rigidity, a series of excellent specific property such as wear-resistant, corrosion-resistant, show the performance advantage of comprehensive beyond tradition particle enhanced aluminum-based composite material, its industrial applications prospect represents gradually, receives very big concern.Research shows, the carbon nanotube of 2-5wt% adds, and its reinforced effects can reach the reinforced effects of the SiC ceramic particle of 10-20wt%, and its unit elongation still can remain on more than 4%, and now SiC particle reinforce system has not almost had plasticity workability.Current Beyer Co., Ltd has been proposed its business-like carbon nanotube and has strengthened 5083 Al alloy composite (registered trademarks
its tensile strength can reach 700MPa, Young's modulus 80GPa, and intensity can compared with carbon steel, density but only have its 1/3rd.Therefore, carbon nanotube enhanced aluminium-based composite material is the superior aluminum matrix composite of tough over-all properties, is subject to the extensive concern of industry member.
Although theoretical investigation shows that single-root carbon nano-tube has superpower mechanical property, Single Walled Carbon Nanotube tensile strength can up to 200GPa, Young's modulus 1TPa, and the performance of carbon nano tube compound material but reaches far away desired by people.Determine that the carbon nanotube key factor that mechanical property plays in body material comprises: carbon nanotube dispersed, orientation, high-content compound and interface cohesion.Namely outstanding mechanics reinforcement has been considered as since carbon nanotube is found, large quantity research has been carried out in dispersion, compound and interface cohesion field, develop various dispersion complex method, but it is very large to realize carbon nanotube orientation in the composite difficulty always of arranging, although it is partially oriented carbon nanotube wherein can be made to obtain by plastic processing deformation in polymer matrix composites, in metal-base composites, this technique cannot be competent at.
Current carbon nanotube enhanced aluminium-based composite material preparation method has powder metallurgic method, spraying method, hot rolling/hot extrusion, super large viscous deformation processing method, agitating friction welding method, in situ synthesis etc., no matter adopt which kind of method, with carbon nanotube dust raw material for starting point, have to pass through Ball milling, alloying mixing and follow-up sintering or plastic working shaping, carbon nanotube structure is destroyed serious, greatly reduce the performance of carbon nanotube mechanical property.The more important thing is, almost could not relate to carbon nanotube distribution of orientations problem, more cannot design matrix material from internal networking structure.CN102787283A discloses a kind of method that carbon nanotube reinforced copper-base composite material is prepared in powder in tube rolling, carries out hot rolling for obtaining target product with copper powder after being mixed by carbon nanotube after enclosing copper pipe.CN102424920A discloses a kind of in-situ preparation method of micro-nano lamination metal base composite material, at flake aluminum surface in situ carbon nano-tube, then prepares target product by lamination hot rolling.Same, in the technology that aforementioned two patents of invention provide, carbon nanotube is still be randomly dispersed within body material.In addition, current all reports and publication are all without how realizing the ordered arrangement of carbon nanotube in aluminum substrate and the method for network structure design, realize the distribution of orientations of carbon nanotube in matrix metal, be the research work with significant challenge always, still have many Science and Technology problems demand to solve.
Summary of the invention
The object of the invention is to for deficiency of the prior art, a kind of ordered carbon nanotube reinforced aluminum matrix composites and preparation method thereof is provided, it passes through carbon nanotube ordered distribution in aluminum substrate, manual control assembling can be realized and form ordered network structure, give full play to the mechanical property that carbon nanotube one-dimentional structure is superpower, realize strengthening aluminum matrix composite mechanical property, give function modified feature simultaneously and realize carbon nanotube network regulation and control Properties of Aluminum Matrix Composites, development has the structure-function integration matrix material of anisotropy functional performance.
For achieving the above object, present invention employs following technical scheme:
A kind of ordered carbon nanotube reinforced aluminum matrix composites, comprises as the aluminium of body material or its alloy and the carbon nanotube that is scattered in order in described body material.
Further, described matrix material comprises 0.01-10wt% carbon nanotube, and wherein carbon nanotube distributes along setting ordered orientation at least partly.
Further say, described matrix material comprises 0.01-10wt% carbon nanotube, at least partly carbon nanotube intersect to form regular network structure with set angle.
Further say, described carbon nanotube is all along single direction ordered distribution.
Further say, described ordered carbon nanotube reinforced aluminum matrix composites is by plural ordered carbon nanotube thin film layer and plural aluminium or the cross layered rear hot rolling of its alloy layer being formed.
As one of comparatively preferred embodiment, wherein at least two-layer adjacent ordered carbon nanotube thin film layer is bent to form by least one continuous print ordered carbon nanotube film.
As one of comparatively preferred embodiment, described ordered carbon nanotube film comprises: arranging as raw material by spinning carbon nano-pipe array, and by super suitable carbon nano-tube film prepared by array membrane technology.
Wherein at least one ordered carbon nanotube thin film layer, the orientation of carbon nanotube is all different from the orientation of carbon nanotube at least another ordered carbon nanotube thin film layer.
A preparation method for ordered carbon nanotube reinforced aluminum matrix composites, comprising: plural ordered carbon nanotube thin film layer and plural aluminium or the cross layered rear hot rolling of its alloy layer are formed described ordered carbon nanotube reinforced aluminum matrix composites; Described ordered carbon nanotube thin film layer is formed by the plural carbon nanotube of ordered distribution.
Further, described ordered carbon nanotube thin film layer is formed by the plural carbon nanotube along setting distribution of orientations, or described ordered carbon nanotube thin film layer comprises the regular network structure intersected to form with set angle by plural carbon nanotube.
Further, the method comprise the steps: by plural ordered carbon nanotube thin film layer and plural aluminium or its alloy layer cross layered after, Vacuum Package in sheath material, then in 350-600 DEG C through the above hot-roll forming of two passages.
Compared with prior art, advantage of the present invention is at least:
(1) by by carbon nanotube ordered arrangement in aluminum substrate, be conducive to the performance advantage giving full play to carbon nanotube one-dimentional structure, obtain significant mechanics and strengthen, overcome the deficiency of disordered carbon nanotube, develop its anisotropy calorifics and electric property application;
(2) by hot rolling technique, ordered carbon nanotube film and the hot rolling of aluminium foil lamination are prepared into matrix material, high-temperature residence time is short, there is process efficient, continuous print feature, can effectively control aluminum substrate and carbon nanotube high-temperature interface reacts, and avoid the violent destruction to carbon nanotube structure in powder metallurgic method mechanical milling process; Meanwhile, prepare carbon nanotube enhanced aluminium-based composite material based on lamination hot rolling technology and there is important mass-producing development & application value.
(3) by by organized carbon nano film multi-angle crossing stack, the aluminum matrix composite that ordered network structure strengthens can be prepared, realize the effective modulation to anisotropic properties.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of ordered carbon nanotube reinforced aluminum matrix composites in embodiment 1;
Fig. 2 be embodiment 1-4 obtain the mechanical property figure of ordered carbon nanotube reinforced aluminum matrix composites;
Fig. 3 is embodiment 1,5-7 obtain the mechanical property figure of ordered carbon nanotube reinforced aluminum matrix composites;
Fig. 4 is embodiment 1,8-10 obtain the mechanical property figure of ordered carbon nanotube reinforced aluminum matrix composites.
Embodiment
In view of many defects of prior art, one aspect of the present invention aims to provide a kind of ordered carbon nanotube reinforced aluminum matrix composites, this material is made up of carbon nanotube and aluminium or its alloy, wherein aluminium or its alloy are body material, carbon nanotube is scattered in body material in orderly or regular array, and carbon nanotubes per-cent is 0.01-10%.
Further say, foregoing carbon nanotubes distribution in body material can be along single direction ordered distribution and present any one of arbitrarily angled regular crossover network distribution.
Another aspect of the present invention aims to provide a kind of preparation method of ordered carbon nanotube reinforced aluminum matrix composites, comprising: plural ordered carbon nanotube thin film layer and plural aluminium or the cross layered rear hot rolling of its alloy layer are formed described ordered carbon nanotube reinforced aluminum matrix composites.
As wherein a kind of scheme that can implement, the method can comprise: adopt chemical vapour deposition technique preparation can spinning carbon nano pipe array, directly prepares super suitable carbon nano-tube film by array membrane technology; Be laid on aluminium foil surface subsequently, through repeatedly lamination, vacuum-sealing is in sheath material; Finally, be preheating to certain temperature, prepare fine and close blank by multiple tracks hot rolling, machining is subsequently removed sheath material and is namely obtained target material.
Aforementionedly can spinning carbon nano pipe array preparation method can be realized by any one in following manner:
(1) by physical deposition techniques at smooth substrate surface deposition catalyst Fe, Co or Fe/Co, substrate can be monocrystalline silicon piece, polysilicon chip, silica glass, pottery any one; Subsequently can spinning carbon nano pipe array by chemical vapour deposition technique growth under 500-900 DEG C of high temperature, its carbon source adopted can be any one or arbitrary combination of the organic steam such as the organic gass such as methane, ethene, acetylene, Sweet natural gas or ethanol, benzene, toluene;
(2) by directly catalyzer being passed in 500-900 DEG C of high temperature CVD stove together with carbon source atmosphere, can spinning carbon nano pipe array at substrate surface in-situ deposition, its catalyzer adopted can be organic molysite and the inorganic molysites such as ferrocene, iron trichloride, iron nitrate, and its carbon source adopted can be any one or arbitrary combination of the organic steam such as the organic gass such as methane, ethene, acetylene, Sweet natural gas or ethanol, benzene, toluene.
Certainly, other technology preparation that the ordered carbon nanotube film in the present invention also can adopt those skilled in the art known.
Foregoing carbon nanotubes can be any one of multi-walled carbon nano-tubes, few-wall carbon nanotube and Single Walled Carbon Nanotube.
Aforementioned Aluminum-aluminum alloy aluminum foil thickness 0.1 micron-1000 microns, can be any one or arbitrary combination in the series alloys such as fine aluminium, Al-Si system, Al-Mg system, Al-Cu system, Al-Zn system, Al-Mg system, Al-Mn system, and be not limited thereto.
As one of comparatively preferred embodiment, the lamination of aforementioned ordered carbon nanotube film and aluminium foil from three layers to any number of plies, and with arbitrarily angled crossing stack, can form carbon nanotube ordered network.
As one of comparatively preferred embodiment, preceding method specifically can comprise: sample vacuum-sealing in copper pipe or aluminum pipe after, through repeatedly hot-roll forming, hot-rolled temperature 350-600 DEG C.
Aforementioned sheath material, except the aforementioned copper pipe of employing or aluminum pipe, also can adopt other metal or non-metallic material, and this is that those skilled in the art specifically adjust according to the demand of practical application.
As wherein a kind of typical embodiment, preceding method can comprise: adopt electron beam evaporation at silicon wafer-based bottom sediments alumina transition layer, deposit Fe, Co or Fe/Co composite membrane subsequently as carbon nano pipe array growth catalyst, in tube furnace, adopt CVD to grow subsequently can spinning carbon nano pipe array; The super suitable carbon nano-tube film with different carbon nanotube structure is then prepared by array membrane technology, be laid on aluminium foil surface, because carbon nanotube has huge surface-area, can adsorbed close at aluminium foil surface, multilayer is intersected stacking, by sample vacuum-sealing in aluminum pipe or copper pipe; Then be preheating to certain temperature (350-600 DEG C), prepared by multistage hot deformation, machining obtains fine and close aluminum matrix composite after removing jacket.
In aforementioned preparation process, for obtaining fine and close aluminum matrix composite, in hot rolling technology, preferably control relative reduction more than 50%.
Below in conjunction with accompanying drawing and some embodiments, technical scheme of the present invention is further described.
Embodiment 1 is see Fig. 1, and this carbon nanotube enhanced aluminium-based composite material is preparation method be achieved in that
Step one: adopt electron beam evaporation at silicon wafer-based bottom sediments alumina transition layer, deposit Fe, Co or Fe/Co composite membrane subsequently as carbon nano pipe array growth catalyst, adopting chemical Vapor deposition process to prepare subsequently in tube furnace can spinning carbon nano pipe array; Then obtain super in-line arrangement carbon nano-tube film by solid phase drawing-die technology;
Step 2: super in-line arrangement carbon nano-tube film 1 being laid on thickness is that pure aluminum foil 2 surface of 0.03mm is repeatedly stacking, is cut into the sample being of a size of 15mm × 20mm;
Step 3: be in the copper pipe of 30mm in external diameter 25mm, wall thickness 0.5mm, length by sample vacuum-sealing, carbon nano-tube film and aluminium foil crossing stack are 7 layers, when relative reduction is 50%, roll rotational speed is that the duo mill of 40rpm is at 500 DEG C of hot-roll formings, machined excision sheath material subsequently, final acquisition ordered carbon nanotube film reinforced aluminum matrix composites.
The difference of embodiment 2 the present embodiment and embodiment 1 is, the thick 0.1mm of aluminium foil in step 2.
The difference of embodiment 3 the present embodiment and embodiment 1 is, the thick 0.05mm of aluminium foil in step 2.
The difference of embodiment 4 the present embodiment and embodiment 1 is, the thick 0.01mm of aluminium foil in step 2.
The difference of embodiment 5 the present embodiment and embodiment 1 is, in step 3, crossing stack is 3 layers.
The difference of embodiment 6 the present embodiment and embodiment 1 is, in step 3, crossing stack is 5 layers.
The difference of embodiment 7 the present embodiment and embodiment 1 is, in step 3, crossing stack is 9 layers.
The difference of embodiment 8 the present embodiment and embodiment 1 is, in step 3, rolling temperature is 400 DEG C.
The difference of embodiment 9 the present embodiment and embodiment 1 is, in step 3, rolling temperature is 450 DEG C.
The difference of embodiment 10 the present embodiment and embodiment 1 is, in step 3, rolling temperature is 550 DEG C.
Obtained by embodiment 1-10 technique, the mechanical property, hardness data etc. of carbon nanotube enhanced aluminium-based composite material refers to Fig. 2-4.Ordered carbon nanotube film according to different carbon nanotube structure substitutes the ordered carbon nanotube film of aforesaid carbon nanotube structure, also can obtain close result.
More than illustrate, and the embodiment shown on drawing, the design philosophy surely of the present invention that is limited can not be resolved.Hold in technical field of the present invention identical know the knowledgeable can by technical thought of the present invention with various form improvement change, such improvement and change are interpreted as belonging in protection scope of the present invention.
Claims (8)
1.
a kind of ordered carbon nanotube reinforced aluminum matrix composites, comprise the aluminium as body material or its alloy, it is characterized in that, described matrix material also comprises 0.01-10wt% carbon nanotube, carbon nanotube is scattered in described body material along setting ordered orientation, and described matrix material is by plural ordered carbon nanotube thin film layer and plural aluminium or the cross layered rear hot rolling of its alloy layer being formed, wherein at least two-layer adjacent ordered carbon nanotube thin film layer is bent to form by least one continuous print ordered carbon nanotube film, and the orientation of carbon nanotube is all different from the orientation of carbon nanotube at least another ordered carbon nanotube thin film layer at least one ordered carbon nanotube thin film layer.
2.
ordered carbon nanotube reinforced aluminum matrix composites according to claim 1, is characterized in that, wherein carbon nanotube intersects to form regular network structure with set angle at least partly.
3.
ordered carbon nanotube reinforced aluminum matrix composites according to claim 1, is characterized in that, described ordered carbon nanotube film comprises: arranging as raw material by spinning carbon nano-pipe array, and by super suitable carbon nano-tube film prepared by array membrane technology.
4.
ordered carbon nanotube reinforced aluminum matrix composites according to claim 1, is characterized in that, described aluminium or its alloy layer comprise aluminium foil or the alloy foil that thickness is 0.1 micron-1000 microns.
5.
the preparation method of ordered carbon nanotube reinforced aluminum matrix composites according to any one of claim 1-4, it is characterized in that, comprising: plural ordered carbon nanotube thin film layer and plural aluminium or the cross layered rear hot rolling of its alloy layer are formed described ordered carbon nanotube reinforced aluminum matrix composites;
described ordered carbon nanotube thin film layer is formed by the plural carbon nanotube of ordered distribution.
6.
the preparation method of ordered carbon nanotube reinforced aluminum matrix composites according to claim 5, it is characterized in that, described ordered carbon nanotube film comprises: arranging as raw material by spinning carbon nano-pipe array, and by super suitable carbon nano-tube film prepared by array membrane technology.
7.
the preparation method of ordered carbon nanotube reinforced aluminum matrix composites according to claim 5, it is characterized in that, the method comprise the steps: by plural ordered carbon nanotube thin film layer and plural aluminium or its alloy layer cross layered after, Vacuum Package in sheath material, then in 350-600 DEG C through the above hot-roll forming of two passages.
8.
the preparation method of ordered carbon nanotube reinforced aluminum matrix composites according to claim 5 or 7, it is characterized in that, described aluminium or its alloy layer comprise aluminium foil or the alloy foil that thickness is 0.1 micron-1000 microns, and described aluminium or its alloy comprise any one or two or more combinations in fine aluminium, Al-Si system, Al-Mg system, Al-Cu system, Al-Zn system, Al-Mg system and Al-Mn system alloy.
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| CN105734459B (en) * | 2014-12-12 | 2017-09-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | The preparation method of carbon nanotube enhanced aluminium-based composite material |
| CN104805432A (en) * | 2015-04-01 | 2015-07-29 | 苏州第一元素纳米技术有限公司 | Preparation method of metal/nanocarbon composite |
| CN105648249B (en) * | 2016-03-02 | 2017-05-31 | 昆明理工大学 | A kind of preparation method of carbon nano tube enhanced aluminium base multilayer materials |
| CN106048324A (en) * | 2016-07-13 | 2016-10-26 | 安徽祈艾特电子科技股份有限公司 | Carbon nano tube reinforced aluminum-magnesium composite alloy material for automobile electronic packaging and preparation method of alloy material |
| CN108866369B (en) * | 2017-05-08 | 2020-03-17 | 清华大学 | Three-dimensional porous composite material |
| CN107377618A (en) * | 2017-06-21 | 2017-11-24 | 昆明理工大学 | A kind of preparation method of multilayer carbon nanotube/copper composite strip |
| CN110963523B (en) * | 2018-09-29 | 2021-11-05 | 清华大学 | Nano porous copper loaded copper oxide nanosheet array composite material and preparation method thereof |
| CN111203442A (en) | 2018-11-22 | 2020-05-29 | 清华大学 | Aluminum-based composite material and preparation method thereof |
| CN110322987B (en) * | 2019-07-09 | 2020-08-18 | 山东大学 | Carbon nanotube reinforced multilayer aluminum matrix composite material and preparation method and application thereof |
| CN112030044B (en) * | 2020-08-21 | 2021-09-24 | 武汉轻工大学 | Carbon nano tube reinforced aluminum matrix composite material and preparation method thereof |
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