CN109338167A - A kind of preparation method of carbon nano tube compound material - Google Patents
A kind of preparation method of carbon nano tube compound material Download PDFInfo
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- CN109338167A CN109338167A CN201811230060.7A CN201811230060A CN109338167A CN 109338167 A CN109338167 A CN 109338167A CN 201811230060 A CN201811230060 A CN 201811230060A CN 109338167 A CN109338167 A CN 109338167A
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- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 59
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 49
- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- -1 carbon nano tube compound Chemical class 0.000 title claims abstract description 11
- 239000002131 composite material Substances 0.000 claims abstract description 111
- 239000008187 granular material Substances 0.000 claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 238000000498 ball milling Methods 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 31
- 229910016384 Al4C3 Inorganic materials 0.000 claims abstract description 24
- 239000004411 aluminium Substances 0.000 claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000001192 hot extrusion Methods 0.000 claims abstract description 15
- 239000011159 matrix material Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 3
- 238000001125 extrusion Methods 0.000 claims description 26
- 239000011261 inert gas Substances 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 11
- 238000003701 mechanical milling Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 235000021355 Stearic acid Nutrition 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 9
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 9
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 9
- 239000008117 stearic acid Substances 0.000 claims description 9
- 238000004886 process control Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000713 high-energy ball milling Methods 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims 2
- 229910052786 argon Inorganic materials 0.000 claims 1
- 238000011065 in-situ storage Methods 0.000 abstract description 4
- 239000005543 nano-size silicon particle Substances 0.000 abstract description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910010271 silicon carbide Inorganic materials 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000007780 powder milling Methods 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 235000013339 cereals Nutrition 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000004080 punching Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000002787 reinforcement Effects 0.000 description 3
- ZBZHVBPVQIHFJN-UHFFFAOYSA-N trimethylalumane Chemical compound C[Al](C)C.C[Al](C)C ZBZHVBPVQIHFJN-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
- C22C2026/002—Carbon nanotubes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Alloys Or Alloy Compounds (AREA)
Abstract
The present invention discloses a kind of preparation method of carbon nano tube compound material, belongs to metal-base composites development field；The method of the invention is that ball milling is carried out after mixing carbon nanotube powder with aluminium powder, and Ball-milling Time is 10h ~ 30h, is obtained containing Al4C3Composite granule；Ball milling is carried out after carbon nanotube is mixed with composite granule, it is made to be uniformly dispersed to obtain CNTs-Al in the base after ball milling 2h ~ 10h4C3The composite granule of/Al；By CNTs-Al4C3The cold moudling at room temperature of/Al composite granule, sintering obtains CNTs-Al in an argon atmosphere4C3/ Al Composite Sintering base obtains CNTs-Al after sintered blank is carried out hot extrusion4C3/ Al composite material.Generated in-situ nano silicon carbide aluminium is well combined with aluminum substrate in the method for the invention plays the role of cooperative reinforcing to composite material together with CNTs；Provide a kind of preparation method of novel aluminum matrix composite with excellent combination mechanical performance.
Description
Technical field
The present invention relates to a kind of preparation methods of carbon nano tube compound material, belong to composite material development field.
Background technique
Composite material is the material with powerful vitality answering Development of Modern Science demand and emerging, it by two kinds or
The different material of two or more properties is combined by various process means.Aluminium on production composite material there are many feature,
Such as light weight, density is small, plasticity is good, and aluminum-base composite technology is easily mastered, easy to process etc..In addition, aluminum matrix composite ratio
Intensity and specific stiffness are high, and high-temperature behavior is good, and more resistant to fatigue and more wear resistant, damping capacity is good, and thermal expansion coefficient is low.It is compound with other
Material is the same, it can combine specific mechanics and physical property, to meet the needs of product.Therefore, aluminum matrix composite has become
For one of material most common, most important in metal-base composites.
Since carbon nanotube is found since 1991, people gradually understand excellent physicochemical property possessed by CNTs.CNTs
Tensile strength reach 50~200GPa, Young's modulus is worked as with diamond phase, and intensity is 100 times of steel, density is about 1.2~
2.1g/cm3, only the 1/6~1/7 of steel；CNTs has excellent conduction and heating conduction, and thermal expansion coefficient is low, has very
Broad application prospect is also acknowledged as optimal composite material reinforcement body.But CNTs dispersibility in the base and and Al
The interface cohesion problem of matrix limits the mechanical property of composite material and further applies.In numerous preparation CNT/Al composite woods
In the method for material ball-milling method due to its simple process, flexibly, controllability is widely used by force.
But traditional ball-milling technology structure of carbon nanotube when CNTs generates aluminium carbide with reactive aluminum is often seriously broken
Bad, so that the load transmission effect of carbon nanotube weakens significantly, therefore improving ball-milling technology makes it that can play aluminium carbide more
The load transmission effect of carbon nanotube can be played again by dissipating invigoration effect, for further increasing the mechanical property of aluminum matrix composite
It can be highly beneficial.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of carbon nano tube compound material, specifically includes the following steps:
(1) ball milling is carried out after mixing carbon nanotube powder with aluminium powder, Ball-milling Time is 10 ~ 30h, is obtained containing Al4C3Answer
Close powder；Wherein the quality of carbon nanotube powder is the 1-2wt.% of mixed-powder gross mass；
(2) ball milling is carried out after mixing carbon nanotube with composite granule obtained in step (1), makes it in base after 2 ~ 10h of ball milling
It is uniformly dispersed to obtain CNTs- Al in body4C3The composite granule of/Al；The quality that carbon nanotube powder is wherein newly added is composite powder
The 1-2wt.% of body gross mass；
(3) by CNTs- Al4C3The cold moudling at room temperature of/Al composite granule, sintering obtains CNTs- in an argon atmosphere
Al4C3/ Al Composite Sintering base obtains CNTs-Al after sintered blank is carried out hot extrusion4C3/ Al composite material.
Preferably, the length of step (1) carbon nanotube of the present invention is 10 ~ 30 μm, and diameter is 20 ~ 30 nm, the partial size of aluminium powder
It is 20 ~ 30 μm.
Preferably, in step (1) of the present invention ball milling detailed process are as follows: by carbon nanotube, pure aluminium powder, abrading-ball in indifferent gas
It is placed in ball grinder under body protection, stiffened resin acid is as process control agent；Wherein, ratio of grinding media to material 10:1, drum's speed of rotation are
250r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball mill rotates forward 30min, then suspends 30 min, then again
30min is inverted, so circulation carries out, and adds up 10 ~ 30h of high-energy ball milling.
Preferably, in step (2) of the present invention ball milling detailed process are as follows: by carbon nanotube, contain nanometer Al4C3Particle
Composite granule, abrading-ball are placed in ball grinder under inert gas shielding atmosphere, and stearic acid is added as process control agent；Wherein,
Ratio of grinding media to material is 10:1, and drum's speed of rotation is 250 r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball mill is rotated forward
Then 30 min suspend 30 min, then invert 30 min again, and so circulation carries out, and add up 2 ~ 10 h of ball milling.
Preferably, the cold pressing of composite granule and sintering detailed process in step (3) of the present invention are as follows: by composite granule in room temperature
Under blank is cold-pressed into the pressure of 300MPa, 600 DEG C of sintering 4h under ar gas environment.
Preferably, in step (3) of the present invention hot extrusion detailed process are as follows: by CNTs-Al4C3/ Al Composite Sintering base
450 DEG C are heated in vacuum or inert gas shielding atmosphere heating furnace, and keeps the temperature 2h to ingot blank internal and external temperature uniformity；With
This simultaneously preheats extrusion die；Use the extrusion ratio of 36:1 by sintered blank hot extrusion for composite material.
The present invention prepares CNTs- Al using two step ball-milling methods4C3/ Al composite material generates aluminium carbide in preparation process and receives
Rice grain plays the role of dispersion-strengtherning in the composite, and suitable CNTs, which is added, is dispersed in CNTs in aluminum substrate,
Play the role of load transmission in the composite, nano silicon carbide aluminium is received with carbon in the composite material prepared by two step ball millings
Mitron synergistic effect improves the intensity of composite material.
Beneficial effects of the present invention: CNTs- Al of the present invention4C3/ Al composite material is prepared using two step ball-milling technologies
Make i.e. comprising nano-particle reinforcement mutually again comprising carbon nano-tube fibre reinforced phase in composite material, the two synergistic effect greatly improves
The intensity of composite material；It is single to solve conventional one step ball milling reinforcement, the undesirable problem of performance；It is of the present invention
CNTs- Al4C3/ Al composite material has the excellent performance of high-strength light.
Detailed description of the invention
Fig. 1 is the process flow chart of the method for the invention；
Fig. 2 is CNTs- Al in the present invention4C3The Raman spectrum of/Al composite material；
Fig. 3 is CNTs- Al in embodiment 14C3The transmission electron microscope photo of/Al composite material；
Fig. 4 is CNTs- Al in embodiment 14C3The dimension formula hardness histogram of/Al composite material and fine aluminium；
Fig. 5 is CNTs- Al in embodiment 14C3The tensile property curve of/Al composite material and fine aluminium.
Specific embodiment
With reference to embodiment, the invention will be further described, but protection scope of the present invention is not limited to
The content.
Embodiment 1
The present invention provides a kind of novel C NTs- Al4C3/ Al composite material and preparation method, includes the following steps；
(1) Al is prepared4C3/ Al composite granule: by carbon nanotube (purity 95%, 10 μm) and pure aluminium powder (purity 99.5%, average grain
25 μm of diameter) it is placed in ball grinder under inert gas shielding atmosphere together with a certain number of abrading-balls, wherein carbon nanotube powder
Quality is the 1wt.% of mixed-powder gross mass, and a small amount of stearic acid is added as process control agent；Ratio of grinding media to material is 10:1, ball mill
Revolving speed is 250 r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball mill rotates forward 30 min, then suspends 30
Then min inverts 30 min again, so circulation carries out, and it is anti-that carbon nanotube and pure aluminium powder occur for accumulative high-energy ball milling
Answer in-situ preparation nanometer Al4C3Particle；Contain nanometer Al to obtain4C3The composite granule of particle.
(2) CNTs- Al is prepared4C3/ Al composite granule: by preparation in carbon nanotube (purity 95%, 10 μm) and step (1)
Contain nanometer Al4C3The composite granule of particle is placed in ball grinder under inert gas shielding atmosphere together with a certain number of abrading-balls
In, wherein the quality that carbon nanotube powder is newly added is the 1wt.% of composite granule gross mass, a small amount of stearic acid is added as process
Controlling agent；Ratio of grinding media to material is 10:1, and drum's speed of rotation is 250 r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball milling
Machine rotates forward 30 min, then suspends 30 min, then inverts 30 min again, and so circulation carries out, and adds up ball milling 6 hours；Ball milling
The finely dispersed CNTs- Al of carbon nanotube is obtained later4C3/ Al composite granule.
(3) compacting and sintering of composite granule: with punching block by CNTs-Al4C3/ Al composite granule is at room temperature with 300MPa
Pressure be cold-pressed into 26 × 1.5 mm cylindrical blank of Ф, 600 DEG C of sintering 4h under ar gas environment.
(4) hot extrusion of sintered blank: by CNTs-Al prepared by step (3)4C3Al Composite Sintering base in vacuum or
It is heated to 450 DEG C in inert gas shielding atmosphere heating furnace, and keeps the temperature 2h to ingot blank internal and external temperature uniformity；At the same time,
Internal diameter Ф 28mm extrusion cylinder and 5 mm extrusion dies are preheated；Then extrusion die and extrusion cylinder are assembled, and the ingot blank of heat is fast
Speed is transferred to extrusion cylinder, uses the extrusion ratio of 36:1 by sintered blank hot extrusion for the CNTs-Al of 5 mm of Ф4C3/ Al composite bar.
Its tensile strength is improved compared with fine aluminium with dimension formula hardness, the composite material in the present embodiment as shown in Fig. 4
Hardness is 82HV, and the hardness of fine aluminium is 63HV, and the hardness of composite material improves 19HV than fine aluminium in the present embodiment.Such as attached drawing 5
The tensile strength of composite material in shown the present embodiment is 258MPa, and the tensile strength of fine aluminium is 202MPa, in the present embodiment
The tensile strength of composite material improves 56MPa than fine aluminium.
Embodiment 2
(1) Al is prepared4C3/ Al composite granule: by carbon nanotube (purity 95%, 20 μm) and pure aluminium powder (purity 99.5%, average grain
30 μm of diameter) it is placed in ball grinder under inert gas shielding atmosphere together with a certain number of abrading-balls, wherein carbon nanotube powder
Quality is the 1.5wt.% of mixed-powder gross mass, and a small amount of stearic acid is added as process control agent；Ratio of grinding media to material is 10:1, ball milling
Machine revolving speed is 250 r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball mill rotates forward 30 min, then suspends 30
Then min inverts 30 min again, so circulation carries out, and it is anti-that carbon nanotube and pure aluminium powder occur for accumulative high-energy ball milling
Answer in-situ preparation nanometer Al4C3Particle.Contain nanometer Al to obtain4C3The composite granule of particle；
(2) CNTs- Al is prepared4C3/ Al composite granule: carbon nanotube (purity 95%, 20 μm) is contained with what is prepared in step (1)
There is a nanometer Al4C3The composite granule of particle is placed in ball grinder under inert gas shielding atmosphere together with a certain number of abrading-balls,
In be newly added carbon nanotube powder quality be composite granule gross mass 2wt.%, a small amount of stearic acid is added as process control
Agent；Ratio of grinding media to material is 10:1, and drum's speed of rotation is 250 r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball mill is just
Turn 30 min, then suspend 30 min, then invert 30 min again, so circulation carries out, and adds up ball milling 6 hours.After ball milling
Obtain the finely dispersed CNTs- Al of carbon nanotube4C3/ Al composite granule.
(3) compacting and sintering of composite granule: with punching block by CNTs-Al4C3/ Al composite granule is at room temperature with 300MPa
Pressure be cold-pressed into 26 × 1.5 mm cylindrical blank of Ф, 600 DEG C of sintering 4h under ar gas environment.
(4) hot extrusion of sintered blank: by CNTs-Al prepared by step (3)4C3/ Al Composite Sintering base in vacuum or
It is heated to 450 DEG C in inert gas shielding atmosphere heating furnace, and keeps the temperature 2h to ingot blank internal and external temperature uniformity；At the same time,
Internal diameter Ф 28mm extrusion cylinder and 5 mm extrusion dies are preheated；Then extrusion die and extrusion cylinder are assembled, and the ingot blank of heat is fast
Speed is transferred to extrusion cylinder, uses the extrusion ratio of 36:1 by sintered blank hot extrusion for the CNTs-Al of 5 mm of Ф4C3/ Al composite bar.
CNTs-Al is prepared in the present embodiment4C3/ Al composite hardness is 73HV, tensile strength 243MPa.
Embodiment 3
(1) Al is prepared4C3/ Al composite granule: by carbon nanotube (purity 95%, 30 μm) and pure aluminium powder (purity 99.5%, average grain
20 μm of diameter) it is placed in ball grinder under inert gas shielding atmosphere together with a certain number of abrading-balls, wherein carbon nanotube powder
Quality is the 2wt.% of mixed-powder gross mass, and a small amount of stearic acid is added as process control agent；Ratio of grinding media to material is 10:1, ball mill
Revolving speed is 250 r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball mill rotates forward 30 min, then suspends 30
Then min inverts 30 min again, so circulation carries out, and it is anti-that carbon nanotube and pure aluminium powder occur for accumulative high-energy ball milling
Answer in-situ preparation nanometer Al4C3Particle；Contain nanometer Al to obtain4C3The composite granule of particle；
(2) CNTs- Al is prepared4C3/ Al composite granule: carbon nanotube (purity 95%, 30 μm) is contained with what is prepared in step (1)
There is a nanometer Al4C3The composite granule of particle is placed in ball grinder under inert gas shielding atmosphere together with a certain number of abrading-balls,
In be newly added carbon nanotube powder quality be composite granule gross mass 1.5wt.%, it is excessively program-controlled that a small amount of stearic acid conduct is added
Preparation；Ratio of grinding media to material is 10:1, and drum's speed of rotation is 250 r/min；For the temperature rise for reducing composite granule in mechanical milling process, ball mill
30 min are rotated forward, 30 min are then suspended, then invert 30 min again, so circulation carries out, and adds up ball milling 6 hours.Ball milling it
After obtain the finely dispersed CNTs- Al of carbon nanotube4C3/ Al composite granule.
(3) compacting and sintering of composite granule: with punching block by CNTs-Al4C3/ Al composite granule is at room temperature with 300MPa
Pressure be cold-pressed into 26 × 1.5 mm cylindrical blank of Ф, 600 DEG C of sintering 4h under ar gas environment.
(4) hot extrusion of sintered blank: by CNTs-Al prepared by step (3)4C3/ Al Composite Sintering base in vacuum or
It is heated to 450 DEG C in inert gas shielding atmosphere heating furnace, and keeps the temperature 2h to ingot blank internal and external temperature uniformity；At the same time,
Internal diameter Ф 28mm extrusion cylinder and 5 mm extrusion dies are preheated；Then extrusion die and extrusion cylinder are assembled, and the ingot blank of heat is fast
Speed is transferred to extrusion cylinder, uses the extrusion ratio of 36:1 by sintered blank hot extrusion for the CNTs-Al4C3/Al composite bar of 5 mm of Ф.
CNTs-Al is prepared in the present embodiment4C3/ Al composite hardness is 66HV, tensile strength 232MPa.
Comparative example
(1) by carbon nanotube (purity 95%, 10 μm) and pure aluminium powder (purity 99.5%, 25 μm of average grain diameter) together with a certain number of
Abrading-ball is placed in ball grinder under inert gas shielding atmosphere, and wherein the quality of carbon nanotube powder is mixed-powder gross mass
A small amount of stearic acid is added as process control agent in 2.5wt.%；Ratio of grinding media to material is 10:1, and drum's speed of rotation is 250 r/min；To subtract
The temperature rise of composite granule, ball mill rotate forward 30 min, then suspend 30 min, then invert 30 min again in few mechanical milling process,
So circulation carries out, and adds up high-energy ball milling 30 hours.
(2) compacting and sintering of composite granule: with punching block by the composite granule in (1) at room temperature with the pressure of 300MPa
It is cold-pressed into 26 × 1.5 mm cylindrical blank of Ф, 600 DEG C of sintering 4h under ar gas environment.
(3) hot extrusion of sintered blank: by Composite Sintering base prepared by step (2) in vacuum or inert gas shielding
It is heated to 450 DEG C in atmosphere heating furnace, and keeps the temperature 2h to ingot blank internal and external temperature uniformity；At the same time, by internal diameter Ф 28mm
Extrusion cylinder and 5 mm extrusion dies are preheated；Then extrusion die and extrusion cylinder are assembled, and the ingot blank fast transfer of heat is extremely squeezed
Cylinder, uses the extrusion ratio of 36:1 by sintered blank hot extrusion for the composite bar of 5 mm of Ф.
Mechanics Performance Testing is carried out to by the obtained composite material of single step ball milling, the results showed that its tensile strength is
236MPa, elongation percentage 14.3%.And in embodiment (1) not using the tensile strength of the composite material of two step ball millings preparation
258MPa, elongation percentage 19.5%, this explanation are superior to using the tensile strength and elongation percentage of the composite material of two step ball millings preparation
Composite material prepared by single step ball milling.
Claims (6)
1. a kind of preparation method of carbon nano tube compound material, which is characterized in that specifically includes the following steps:
(1) ball milling is carried out after mixing carbon nanotube powder with aluminium powder, wherein the quality of carbon nanotube powder is that mixed-powder is total
The 1-2wt.% of quality, Ball-milling Time are 10h ~ 30h, are obtained containing Al4C3Composite granule；
(2) ball milling is carried out after mixing carbon nanotube with composite granule obtained in step (1), make after ball milling 2 h ~ 10 h its
It is uniformly dispersed to obtain CNTs- Al in matrix4C3The composite granule of/Al；It is compound that the quality of carbon nanotube powder, which is wherein newly added,
The 1-2wt.% of powder quality；
(3) by CNTs- Al4C3The cold moudling at room temperature of/Al composite granule, sintering obtains CNTs- in an argon atmosphere
Al4C3/ Al Composite Sintering base obtains CNTs-Al after sintered blank is carried out hot extrusion4C3/ Al composite material.
2. the preparation method of carbon nano tube compound material according to claim 1, it is characterised in that: carbon nanometer in step (1)
The length of pipe is 10 ~ 30 μm, and diameter is 20 ~ 30nm, and the partial size of aluminium powder is 20 ~ 30 μm.
3. the preparation method of carbon nano tube compound material according to claim 1, it is characterised in that: ball milling in step (1)
Detailed process are as follows: be placed in carbon nanotube, pure aluminium powder, abrading-ball in ball grinder under inert gas protection, stiffened resin acid was used as
Program-controlled preparation；Wherein, ratio of grinding media to material 10:1, drum's speed of rotation 250r/min；For the temperature for reducing composite granule in mechanical milling process
It rises, ball mill rotates forward 30 min, then suspends 30 min, then inverts 30 min again, and so circulation carries out, and adds up high-energy ball milling
10~30h。
4. the preparation method of carbon nano tube compound material according to claim 1, it is characterised in that: ball milling in step (2)
Detailed process are as follows: by carbon nanotube, contain nanometer Al4C3Composite granule, the abrading-ball of particle are placed under inert gas shielding atmosphere
In ball grinder, stearic acid is added as process control agent；Wherein, ratio of grinding media to material 10:1, drum's speed of rotation are 250 r/min；For
The temperature rise of composite granule in mechanical milling process is reduced, ball mill rotates forward 30 min, then suspends 30 min, then invert 30 again
Min, so circulation are carried out, and add up 2 ~ 10h of ball milling.
5. the preparation method of carbon nano tube compound material according to claim 1, it is characterised in that: composite powder in step (3)
The cold pressing and sintering detailed process of body are as follows: composite granule is cold-pressed into blank at room temperature with the pressure of 300MPa, in argon gas ring
The lower 600 DEG C of sintering 4h in border.
6. the preparation method of carbon nano tube compound material according to claim 1, it is characterised in that: hot extrusion in step (3)
Detailed process are as follows: by CNTs-Al4C3/ Al Composite Sintering base heats in vacuum or inert gas shielding atmosphere heating furnace
To 450 DEG C, and 2h is kept the temperature to ingot blank internal and external temperature uniformity；Extrusion die is preheated at the same time；Using squeezing for 36:1
Sintered blank hot extrusion is composite material by pressure ratio.
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