CN107227417A - A kind of method for preparing carbon nanotube reinforced copper-base composite material - Google Patents
A kind of method for preparing carbon nanotube reinforced copper-base composite material Download PDFInfo
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- CN107227417A CN107227417A CN201710278601.2A CN201710278601A CN107227417A CN 107227417 A CN107227417 A CN 107227417A CN 201710278601 A CN201710278601 A CN 201710278601A CN 107227417 A CN107227417 A CN 107227417A
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- copper
- carbon nanotube
- composite material
- base composite
- nanotube reinforced
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- 239000002131 composite material Substances 0.000 title claims abstract description 68
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 47
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 36
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052802 copper Inorganic materials 0.000 claims abstract description 33
- 239000010949 copper Substances 0.000 claims abstract description 33
- 230000006698 induction Effects 0.000 claims abstract description 19
- 238000007493 shaping process Methods 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 230000002708 enhancing effect Effects 0.000 claims abstract description 8
- 238000005096 rolling process Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000000758 substrate Substances 0.000 abstract description 9
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 5
- 238000000713 high-energy ball milling Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000004663 powder metallurgy Methods 0.000 abstract description 4
- 238000007789 sealing Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 13
- 239000008187 granular material Substances 0.000 description 12
- 208000010392 Bone Fractures Diseases 0.000 description 11
- 206010017076 Fracture Diseases 0.000 description 11
- 239000000463 material Substances 0.000 description 5
- 238000005245 sintering Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 206010068052 Mosaicism Diseases 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 210000003765 sex chromosome Anatomy 0.000 description 2
- 208000006670 Multiple fractures Diseases 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007596 consolidation process Methods 0.000 description 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000000754 repressing effect Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- 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
- C22C9/00—Alloys based on copper
-
- 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
Abstract
The present invention discloses a kind of method for preparing carbon nanotube reinforced copper-base composite material, specifically comprises the steps of：By CNT and copper powder according to mass ratio 82 ~ 199:After 1 ratio ball milling, it is fitted into compacting and sealing two ends in copper pipe；Copper pipe is sent into shaping of swaging is carried out in the swager with radio-frequency induction coil, the shaping of swaging for mould of being swaged by multi-pass different-diameter obtains rod carbon nanotube enhancing Cu-base composites；Present method solves the interfacial bonding property of prior powder metallurgy preparation technology flow very complicated, CNT and Copper substrate and it is uniformly dispersed the problem of, using high-energy ball milling batch mixing and the forming method for sensing heating of swaging, better than the batch mixing and moulding process of prior powder metallurgy, the technological process is simple, efficient energy-saving is beneficial to industrialization production.
Description
Technical field
The invention belongs to field of metal matrix composite, more particularly to one kind prepares carbon nanotube reinforced copper-base composite material
Preparation method.
Background technology
Carbon nanotube reinforced copper-base composite material is by the electric property of the high conductivity of copper and the high resiliency mould of CNT
Amount, high intensity, the advantage of the mechanical property of high abrasion rolls into one, and breaches copper metal because self-strength can not enough expire
Sufficient high abrasion, the limitation of the harsher application conditions of high-tensile makes it in bullet train arch slide plate, switch electric contact
Material, and the high-end electric and electronic field such as precision circuit support lead are with a wide range of applications.
The preparation method of current carbon nanotube reinforced copper-base composite material is mainly the method using powder metallurgy, specific mistake
Journey is to first pass through different methods composite granule is made, then by composite granule using consolidation sides such as vacuum hotpressing, plasma agglomerations
Carbon nanotube reinforced copper-base composite block material is made in formula sinter molding.It is wherein derivative according to the preparation method of composite granule difference
Go out electroless plating method, molecular level mixing, in-situ synthesis, agitating friction method, high-energy ball milling method etc..Byung K. Lim are by changing
Learn the carbon nanotube reinforced copper-base composite material that plating plasma agglomeration obtains 15vol%, electrical conductivity 72%IACS, tensile strength
341.2MPa.CNT and copper powder high-energy ball milling mixing hot repressing sintering are obtained composite material tensile strength by Shukla.A.K
For 330MPa.Cha and Kim is obtained surface-functionalized carbon pipe and copper acetate mixing-hydrogen reducing using molecular level mixing method
Carbon nanotube reinforced copper-base composite material is obtained to composite granule, then plasma agglomeration, tensile strength reaches 360MPa compared with fine copper
Improve 230%.A kind of patent CN201210095598.8 " preparation method of carbon nanotube reinforced copper-base composite material " inventor
Cai Xiaolan, the patent uses high-energy ball milling method batch mixing, CNT enhancing prepared by annealing-cold pressing-sintering and moulding technology scheme
Cu-base composites, CNT is uniformly dispersed in the base, but its moulding process flow process is longer, resulting composite
Electric conductivity lifting is limited.
The problem of being primarily present at present around carbon nanotube reinforced copper-base composite material is the boundary of CNT and Copper substrate
Face associativity and dispersed sex chromosome mosaicism, prepare carbon nanotube reinforced copper-base using traditional powder metallurgy process in addition and are combined
Material movement very complicated, therefore exploitation sends as an envoy to carbon pipe and matrix is uniformly dispersed, interface cohesion is good and production procedure is simple
Preparation method be promote nanotube strengthen Cu-base composites broader applications key.
The content of the invention
The present invention provides a kind of preparation method for preparing carbon nanotube reinforced copper-base composite material, and the preparation method is simple simultaneously
And flow is short, carbon pipe distributing homogeneity and interface cohesion sex chromosome mosaicism in Copper substrate can not only be solved, moreover it is possible to meet industrialization company
The problem of continuous batch production, the preferable high-performance carbon nanotube enhancing Cu-base composites of tensile strength and conductance are made,
And it is suitable for industrialization production.
A kind of method for preparing carbon nanotube reinforced copper-base composite material, specifically includes following steps：
（1）By CNT and copper powder according to mass ratio 1:After 80-200 ratio ball milling, it is fitted into compacting and two in copper pipe
End closure；
（2）By step（1）Swager of the copper pipe feeding with radio-frequency induction coil in swage shaping, by multi-pass not
Swaged with diameter the shaping of swaging of mould, obtain rod carbon nanotube enhancing Cu-base composites.
Step（1）The rotational speed of ball-mill is 500-700r/min, and Ball-milling Time is 60min.
Step（2）The copper pipe feeding speed is 10-50cm/min.
Step（2）The heating-up temperature of the radio-frequency induction coil is 550-750 DEG C.
Step（2）The rolling pass of the shaping of swaging is 2-10 times.
Step（2）The radio-frequency induction coil is arranged on the outside swaged in swager.
Beneficial effects of the present invention：
（1）The heating of radio-frequency induction coil and combination of swaging, the three-dimensional pressure that the medium and small deformed area of deformation of swaging repeatedly forges generation should
Force deformation, it is final to realize very big deflection, beneficial to CNT in Copper substrate it is dispersed and between Copper substrate
Interface cohesion, increase CNT and Copper substrate bond strength, crystal grain thinning, improve CNT directionality make its axial direction
Arrangement, beneficial to consistency, tensile strength and the electrical conductivity for improving composite, itself adds along with swaging to composite
Work induration, the mechanical property and electric conductivity of obtained Carbon Nanotubes Reinforced Composites is stable.
（2）This method flow is short, and technique is simple, is continuously produced beneficial to industrialization, and swage composite when material sheet
Body can produce heat so that additional forming temperature can be reduced, short the time required to whole forming process, save energy consumption, nothing
Gas and solid waste are produced it is achieved thereby that the target of green production.
Brief description of the drawings
Fig. 1 is that the present invention swages sensing heating shaped device part-structure schematic diagram；
Fig. 2 be the embodiment of the present invention 1 swage sensing heating preparation rod carbon nanotube enhancing Cu-base composites；
Fig. 3 for the embodiment of the present invention 3 composite CNT and Copper substrate interface cohesion TEM patterns；
Fig. 4 is the metallographic SEM patterns of the embodiment of the present invention 3 and comparative example composite：（a）The metallographic SEM patterns of comparative example；
（b）The metallographic SEM patterns of embodiment 3；
Fig. 5 is the composite fracture apperance of the embodiment of the present invention 3：（a）2000 fracture apperances of embodiment 3；（b）Embodiment 3
8000 times of fracture apperances；
Fig. 6 is the composite fracture apperance of comparative example of the present invention：（a）2000 fracture apperances of comparative example；（b）Comparative example
8000 times of fracture apperances；
In figure, 1- copper pipes, 2- radio-frequency induction coil temperature controllers, 3- radio-frequency induction coils, 4- swages mould, 5- swagers.
Embodiment
According to following instance, it will be further appreciated that of the invention, still, those skilled in the art is readily appreciated that implementation
Specific formula, proportioning, technological parameter, condition and result described in example are merely to illustrate the present invention, without that should be able to limit power
The present invention being described in detail in sharp claim.
Embodiment 1
A kind of method for preparing carbon nanotube reinforced copper-base composite material of the present embodiment, specifically includes following steps：
（1）2.5g CNTs and 497.25g 600 mesh copper powders are added in high energy ball mill, with 500r/min alternation rotating speeds
Ball milling 60min obtains well mixed carbon nanotube reinforced copper-base composite granule, is 0.5mm, outside by composite granule loading wall thickness
Footpath 10mm, length are compacting and sealing two ends in 0.3m copper pipe；
（2）By step（1）Copper pipe 10cm/min the internal swager with radio-frequency induction coil of speed feeding in revolved
Forging molding, as shown in figure 1, radio-frequency induction coil is arranged on the outside swaged in swager, the heating temperature of radio-frequency induction coil
Spend for 550 DEG C, the shaping of swaging for mould of being swaged successively according to diameter 8mm, 6mm mould 2 passage different-diameters of progress is subtracted
Mass runoff is the 40% i.e. rod carbon nanotube enhancing Cu-base composites of 0.55 meter of length of a diameter of 6mm or so, as shown in Figure 2.
Embodiment 2
A kind of method for preparing carbon nanotube reinforced copper-base composite material of the present embodiment, specifically includes following steps：
（1）20g CNTs and 2980g 600 mesh copper powders are added in high energy ball mill, with 600r/min alternation rotating speed balls
Mill 60min obtains well mixed carbon nanotube reinforced copper-base composite granule, and it is 5.0mm, external diameter that composite granule is loaded into wall thickness
60mm, length are compacting and sealing two ends in 2m copper pipe；
（2）By step（1）Copper pipe to be carried out in the internal swager with radio-frequency induction coil of 50cm/min speed feeding
Swage shaping, radio-frequency induction coil is arranged on the outside swaged in swager, and the heating-up temperature of radio-frequency induction coil is 750
DEG C, carry out 10 according to diameter 54mm, 48mm, 42mm, 36mm, 30mm, 24mm, 18mm, 16mm, 14mm, 12mm mould successively
Passage different-diameter is swaged the shaping of swaging of mould, and it is the bar-shaped of 80% i.e. a diameter of 12mm or so 3.1 meters of length to obtain deflection
Carbon nanotube reinforced copper-base composite material.
Embodiment 3
A kind of method for preparing carbon nanotube reinforced copper-base composite material of the present embodiment, specifically includes following steps：
（1）12.04g CNTs and 987.96g 600 mesh copper powders are added in high energy ball mill, turned with 700r/min alternations
Fast ball milling 60min obtains well mixed carbon nanotube reinforced copper-base composite granule, be 1.0mm by composite granule loading wall thickness,
External diameter 20mm, length are compacting and sealing two ends in 1 m copper pipe；
（2）By step（1）Copper pipe to be carried out in the internal swager with radio-frequency induction coil of 30cm/min speed feeding
Swage shaping, radio-frequency induction coil is arranged on the outside swaged in swager, and the heating-up temperature of radio-frequency induction coil is 650
DEG C, carry out 5 passage different-diameters according to diameter 18mm, 16mm, 14mm, 12mm, 10mm mould successively and swage the swaging of mould
Shaping, obtains rod carbon nanotube enhancing Cu-base composites of the deflection for 50% i.e. a diameter of 10mm or so 2.5 meters of length；
Fig. 3 is the TEM shape appearance figures of the carbon nanotube reinforced copper-base composite material of embodiment 3, it can be seen that carbon pipe is in Copper substrate
It is middle closely to be surrounded, and intermediate transition zone is without obvious boundary line, illustrates that the interface cohesion of CNT and Copper substrate is good.
Comparative example
A kind of method for preparing carbon nanotube reinforced copper-base composite material of the present embodiment, specifically includes following steps：
（1）12.04g CNTs and 987.96g 600 mesh copper powders are added in high energy ball mill, turned with 700r/min alternations
Fast ball milling 60min obtains well mixed carbon nanotube reinforced copper-base composite granule.
（2）Composite granule is passed through into traditional vacuum heating-press sintering, 850 DEG C of sintering temperature, sintering pressure 70MPa, pressurize
1h obtains carbon nanotube reinforced copper-base composite material.
Fig. 4 is the metallographic SEM patterns contrast of composite obtained by embodiment 3 and comparative example, it can be seen that this reality
The average grain size for applying the carbon nanotube reinforced copper-base composite material that example is obtained is about less than 10 μm, and this is more compound than comparative example
The crystallite dimension of material（More than about 20 μm）It is much smaller, illustrate that the technique of embodiment 3 is obtained for the crystal grain of refining composite material
Beneficial effect；Fig. 5 is the composite fracture apperance of embodiment 3, and Fig. 6 is that the composite in comparative example amplifies same multiple
Fracture apperance, it is apparent that typical ductile rupture shape is presented in the fracture apperance of embodiment 3 from the contrast of fracture apperance
Looks, CNT is arranged vertically, and comparative example presents the fracture apperance of Brittle cleavage fracture, and embodiment 3 is illustrated well
Process improving CNT directionality make its axial arranging.
The composite material surface that comparative example is obtained polishes flat smooth, and the composite that embodiment 1-3 is obtained is using same
Outside copper pipe is polished clean by the technique of sample, and its consistency, electronic universal tester 0.5mm/min speed are determined using real density instrument
Degree determines its tensile strength, and vortex conductivity apparatus determines its electrical conductivity, and specific detection data see the table below 1.
Table 1 is composite consistency, tensile strength, the experimental data of electrical conductivity prepared by comparative example and embodiment.
As shown in Table 1, the consistency for the carbon nanotube reinforced copper-base composite material that embodiment 1-3 is obtained, tensile strength, electricity
Conductance be intended to than in comparative example using traditional vacuum hot pressing formation carbon nanotube reinforced copper-base composite material good compactness,
Tensile strength is improved, electrical conductivity is improved, and this illustrates that the method for the invention can significantly improve carbon nanotube reinforced copper well
Based composites consistency, tensile strength, electrical conductivity.
Claims (6)
1. a kind of method for preparing carbon nanotube reinforced copper-base composite material, it is characterised in that specifically comprise the steps of：
（1）By CNT and copper powder according to mass ratio 1:After 80-200 ratio ball milling, it is fitted into compacting and two in copper pipe
End closure；
（2）By step（1）Swager of the copper pipe feeding with radio-frequency induction coil in swage shaping, by multi-pass not
Swaged with diameter the shaping of swaging of mould, obtain rod carbon nanotube enhancing Cu-base composites.
2. the method for carbon nanotube reinforced copper-base composite material is prepared according to claim 1, it is characterised in that step（1）
The rotational speed of ball-mill is 500-700r/min, and Ball-milling Time is 60min.
3. the method for carbon nanotube reinforced copper-base composite material is prepared according to claim 1, it is characterised in that step（2）
The copper pipe feeding speed is 10-50cm/min.
4. the method for carbon nanotube reinforced copper-base composite material is prepared according to claim 1, it is characterised in that step（2）
The heating-up temperature of the radio-frequency induction coil is 550-750 DEG C.
5. the method for carbon nanotube reinforced copper-base composite material is prepared according to claim 1, it is characterised in that step（2）
The rolling pass of the shaping of swaging is 2-10 times.
6. the method for carbon nanotube reinforced copper-base composite material is prepared according to claim 1, it is characterised in that step（2）
The radio-frequency induction coil is arranged on the outside swaged in swager.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710278601.2A CN107227417A (en) | 2017-04-25 | 2017-04-25 | A kind of method for preparing carbon nanotube reinforced copper-base composite material |
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| CN201710278601.2A CN107227417A (en) | 2017-04-25 | 2017-04-25 | A kind of method for preparing carbon nanotube reinforced copper-base composite material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108118174A (en) * | 2017-12-29 | 2018-06-05 | 中南大学 | A kind of preparation method of carbon nanotube reinforced copper-base composite material |
| CN109851385A (en) * | 2019-01-25 | 2019-06-07 | 西南交通大学 | A kind of hydroxyl functional carbon nano tube enhancing pantograph pan and preparation method thereof |
| CN111462938A (en) * | 2020-04-17 | 2020-07-28 | 珠海蓉胜超微线材有限公司 | Copper-coated carbon nano composite flat wire and preparation method thereof |
| CN112453385A (en) * | 2020-11-23 | 2021-03-09 | 成都威士达粉末冶金有限公司 | Powder metallurgy composite material with high composite ratio and manufacturing method thereof |
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| CN101876019A (en) * | 2009-12-11 | 2010-11-03 | 中南大学 | Die material for copper hot extrusion and preparation process thereof |
| CN102628115A (en) * | 2012-04-01 | 2012-08-08 | 昆明理工大学 | Preparation method of carbon nano tube enhanced copper-based composite material |
| JP2013505353A (en) * | 2009-09-17 | 2013-02-14 | バイエル・マテリアルサイエンス・アクチェンゲゼルシャフト | Composite materials containing metals and nanoparticles |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108118174A (en) * | 2017-12-29 | 2018-06-05 | 中南大学 | A kind of preparation method of carbon nanotube reinforced copper-base composite material |
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| CN109851385A (en) * | 2019-01-25 | 2019-06-07 | 西南交通大学 | A kind of hydroxyl functional carbon nano tube enhancing pantograph pan and preparation method thereof |
| CN109851385B (en) * | 2019-01-25 | 2021-01-26 | 西南交通大学 | Hydroxyl-functionalized carbon nanotube-reinforced pantograph slide plate and preparation method thereof |
| CN111462938A (en) * | 2020-04-17 | 2020-07-28 | 珠海蓉胜超微线材有限公司 | Copper-coated carbon nano composite flat wire and preparation method thereof |
| CN112453385A (en) * | 2020-11-23 | 2021-03-09 | 成都威士达粉末冶金有限公司 | Powder metallurgy composite material with high composite ratio and manufacturing method thereof |
| CN112453385B (en) * | 2020-11-23 | 2022-09-27 | 成都威士达粉末冶金有限公司 | Powder metallurgy composite material with high composite ratio and manufacturing method thereof |
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