CN106350695A - Preparation method of elemental-copper-coated multiwalled carbon nanotube/aluminum-based composite semisolid-state blank - Google Patents
Preparation method of elemental-copper-coated multiwalled carbon nanotube/aluminum-based composite semisolid-state blank Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/12—Making non-ferrous alloys by processing in a semi-solid state, e.g. holding the alloy in the solid-liquid phase
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1005—Pretreatment of the non-metallic additives
- C22C1/101—Pretreatment of the non-metallic additives by coating
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C21/00—Alloys based on aluminium
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
- C22C47/04—Pretreatment of the fibres or filaments by coating, e.g. with a protective or activated covering
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/04—Light metals
- C22C49/06—Aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
Abstract
A preparation method of an elemental-copper-coated multiwalled carbon nanotube/aluminum-based composite semisolid-state blank includes: preparing an elemental-copper-coated multiwalled carbon nanotube; guiding aluminum alloy powder and the elemental-copper-coated multiwalled carbon nanotube into a ball milling crucible, and performing ball milling treatment under protection of argon; putting mixed powder into the crucible, using a muffle furnace to heat to 20-40 DEG C below a solid-phase line, transferring into an ultrasonic magnetic stirring furnace, continuing heating, controlling solid-phase rate to a certain range, vibrating and stirring at a low speed, feeding argon for protection, and controlling stirring time; pouring obtained size into a corresponding die, and cooling to obtain the semisolid-state blank. The preparation method has the advantages of simplicity, safety, low cost, easiness in operation and controllability.
Description
Technical field
The invention belongs to technical field of material.
Background technology
In recent years, using fiber or granule, aluminium alloy is carried out with composite strengthening, the aluminum matrix composite of preparation is high due to it
Specific strength, the advantages of good electrical and thermal conductivity performance and low thermal coefficient of expansion, attracted very big to pay close attention to and be widely used in navigating
Its aviation, automobile making, the field such as electronic machine.
CNT is hollow nano structure, the envelope by the tube of graphite hexagonal network curling with uniqueness
The topology configuration closing and helical structure, thus having excellent properties special in a large number, such as high intensity, high resiliency, high-specific surface area,
Heat-resisting, corrosion-resistant, heat conduction and electric conductivity etc., imply CNT has huge application space in materials application research.Carbon
The modulus of nanotube is identical with diamond, and theoretical strength has reached 106MPa, it is 100 times of iron and steel, and density is only iron and steel
1/6, it has both extremely excellent toughness and structural stability again simultaneously, is the ideal chose strengthening phase as composite.Right cnt's
Defect is also apparent.Carbon pipe is due to its stable sp2Structure, shows the wettability of extreme difference simultaneously, CNT is in founding
During easily reunite and wrapping phenomena causes not strong with metallic matrix interfacial bonding property, be unfavorable for the increasing of composite property
By force.Therefore, how to reduce agglomeration in Metal Forming Process for the CNT, and improve it is become with the wettability of matrix
The key of the excellent carbon nano-tube reinforced metal-matrix composite material of processability.
CNT improves wettability method at present overlay coating etc., such as chemical nickel plating, and the method mainly will complete base
The CNT changed, through sensitization plays, after activation, puts into plating in chemical plating fluid, and the carrying out with reaction can be in carbon nano tube surface
Obtain continuous, uniform coating, but expensive, and commonly use toxic reagent, not environmentally and production cost is high, be not suitable for advising greatly
Mould produces.Sol method is also popular research coating direction, adds organic compound in the solution and stirs, reaction a period of time,
It is subsequently adding CNT, add acid group metallic compound to be kept stirring for state until generating colloidal sol, this colloid is exposed to sky
Aging in gas, after a few days product grind into powder is dried, in last uniform temperature inert gas flow, heat treatment obtains for a period of time
To nano-complex particle.But the proportioning difficulty of amount is big, and the response time is long.
In publication number cn101966449a, entitled: " for a kind of system of multiwall carbon nanotube-supported titanium dioxide catalyst
In Preparation Method ".Solvent thermal and hydro-thermal method are combined, adsorbs colloid in a solvent, be dried in carbon nano tube surface, hydro-thermal is divided
Solve its colloid, obtain aoxidizing applicator.So the method step is complicated, and the time is long, and can not coat simple substance in CNT table
Face, has certain limitation.
On the other hand, the control to CNT dispersibility is generally embodied in metal preparation process.At present, by stirring
It is relatively conventional that casting, in-situ synthesis and powder metallurgic method prepare the strong aluminum matrix composite of CNT.But this several side
The defect of method is also it is clear that CNT is reunited seriously with the flowing of melt under casting condition, strengthens distributed mutually uneven
Even, powder metallurgy is popular research direction, but interface cohesion and fine and close sex chromosome mosaicism fail to obtain effectively solving.In-situ synthesis
There is technique excessively complexity and process is difficult to the short slabs such as control.
In publication number cn103614672a, entitled " preparation method of carbon nanotube enhanced aluminium-based composite material ", adopt
With batch mixing, drying, ball milling, the conventional powder metallurgical method such as colding pressing, sinter and extrude, to be prepared for carbon nano tube enhanced aluminium base multiple
Condensation material, right interfacial bonding property is poor, more prominent the problems such as the compactness of material itself.
In publication number cn103911566a, a kind of entitled " powder metallurgy of carbon nano tube reinforced aluminum alloy composite material
In preparation method ", more uniform by CNT using powder metallurgy process process flake aluminum, but conventional powder metallurgical side
The defect of method does not such as melt, and not good etc. defect of compactness does not solve.
In publication number cn101376932, entitled " CNT strengthens magnesium, aluminum matrix composite and preparation method thereof "
In, CNT is prepared using mixing reho-forming method after powder heating and strengthens aluminum, magnesium base composite material.Though densification can be improved
Sex chromosome mosaicism, but under rheological condition, CNT is easily reunited, and the performance raising to composite is unfavorable.
Therefore, still lack a kind of cost-effective carbon nanotube enhanced aluminium-based composite material preparation at present and shape skill
Art.
In order to overcome traditional carbon nano tube compound material to be prepared into the technological difficulties of type, the invention is intended to providing a kind of new
CNT/alumina-base material semi-solid blank preparation forming technique.Semi-solid state forming technique comes across 20 century 70s, this work
Skill, as a kind of efficient, energy-conservation modern metallurgical technology, achieves over nearly 40 years and develops rapidly, range of application constantly expands.It
With respect to forming technologies such as conventional cast and forgings, there are several obvious advantages: reduce gross segregation and the cavity of finished product, less
Forming pressure, and relatively low mold temperature etc..Just because of this technology has a series of particular advantages thus extremely common people look steadily
Mesh, also will become this century the most potential material forming techniques.
Semi-solid state forming technique includes the preparation of semi-solid blank, the post bake of blank and the crucial ring of thixotropic forming 3
The preparation of section, wherein semi-solid blank is core the most.It directly influences subsequent technique and final product quality.
Content of the invention
The purpose of the present invention is to propose to a kind of simple substance copper clad multi-walled carbon nano-tubes/aluminum matrix composite semi-solid blank
Preparation method.
The present invention is achieved by the following technical solutions.
A kind of preparation side of simple substance copper clad multi-walled carbon nano-tubes/aluminum matrix composite semi-solid blank of the present invention
Method, comprises the following steps.
(1) by multi-walled carbon nano-tubes in the ultrasonic pre-dispersed 6 ~ 8h of pure salpeter solution, temperature is 60 ~ 80 DEG C, is cooled to room temperature
Afterwards, deionized water cleaning, is centrifuged to neutrality, then dries in vacuum drying oven, standby.
(2) multi-walled carbon nano-tubes by copper nitrate with through step (1) pretreatment is added in ethanol solution, ultrasonic 40～
60min, obtains carbon nanotube suspension, wherein multi-walled carbon nano-tubes and copper nitrate mol ratio 1:0.4～1:1.
(3) the multi-walled carbon nano-tubes suspension through step (2) is imported in hydrothermal reaction kettle, wherein suspension volume accounts for
Reactor molten long-pending 25%～50%.Place into heating in reacting furnace, be warming up to 180～200 DEG C with 1～5 DEG C/s, be incubated 1～2h, then
It is warming up to after 300 DEG C with 1～5 DEG C/s, be incubated 8～12h；Take out, reactor seals air cooling, dried with vacuum drying oven, obtain prefabricated
Material.
(4) put into vacuum tube furnace after putting in corundum crucible through step (3) gained mixing material, 300 ~ 500 DEG C high
Warm roasting 3 hours, obtains the many walls nanotube material of simple substance copper clad.
(5) the many walls nanotube material of the simple substance copper clad that step (4) is obtained is mixed with Al alloy powder, puts into ball milling earthenware
Crucible carries out ball milling, and time control accounts for Al alloy powder in 30 ~ 60min, the many walls nanotube quality of materials of wherein simple substance copper clad
2% ~ 4%, this process is passed through argon and is protected.
(6) step (5) gained mixed-powder is put in crucible, with muffle furnace with 5 ~ 10 DEG C/min heating rate extremely
After 10 ~ 20 DEG C of subsolidus, proceed in ultrasonic magnetic agitation stove and continue to heat and control its solid rate in 20 with 1 ~ 3 DEG C/min
~ 40% scope, ultrasonic should be indirectly ultrasonic, power pass through crucible bottom incoming.And Power Control is in 1.0 ~ 2.0kw, frequency
20khz, stirring at low speed is simultaneously passed through argon protection, and ultrasonic magnetic agitation time control is in 1 ~ 3min.
(7) step (6) gained semi solid slurry is poured into corresponding mould cooling, obtain simple substance copper clad multi-wall carbon nano-tube
Pipe/aluminum matrix composite semi-solid blank.
Hydrothermal reaction kettle liner described in step (3) of the present invention is politef.
In the present invention, using ultrasonic and magnetic stirring equipment synergism, mixed under concussion stirring semi-molten state
Close powder, not only can promote the dispersion of cnt, the reunion of cnt, agglomerating and rising phenomenon can be reduced simultaneously.
The concrete principle of the present invention is:
2cu(no3)2=2cuo+4no2+o2(1)
ch3ch2oh + cuo = ch3cho + cu + h2O (2)
Under high temperature, copper nitrate decomposes, and recycles the further reduction treatment of catalysis activity of copper oxide, obtains copper simple substance carbon coated and receive
Nanotube material.Pretreated CNT is mixed with alloyed powder, carries out stirring at low speed in semi-solid temperature interval, controls solid phase
Rate to be incubated special time long, obtains required semi-solid blank.
The present invention has following uniqueness: (1) the method reduces the rising phenomenon of cnt in common process.(2) using this
The oxide that body copper nitrate decomposes in a heated condition is catalyzed further and is reduced into elemental copper and is deposited directly on whisker.(3)
The method reaction temperature is relatively low, and danger coefficient is low.(4) multi-walled carbon nano-tubes is combined with matrix under the conditions of aluminium alloy semi-solid,
While there is more preferable interface, further reduce the reunion probability of CNT under founding state.
Brief description
Fig. 1 is the semi-solid blank microscopic structure of preparation in embodiment 1.
Specific embodiment
The present invention will be described further by following examples.
Embodiment 1.
By multi-walled carbon nano-tubes in the ultrasonic pre-dispersed 8h of pure salpeter solution, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleans, is centrifuged to neutrality, then in vacuum drying oven dry for standby.The multi-walled carbon nano-tubes of copper nitrate and above-mentioned drying is made
For raw material, add ultrasonic 40min in straight alcohol；Wherein multi-walled carbon nano-tubes, copper nitrate and ethanol mol ratio are 1:0.4:127,
Obtain multi-walled carbon nano-tubes suspension；This suspension is imported in hydrothermal reaction kettle, wherein to account for reactor molten long-pending for suspension volume
25%.Place into heating in reacting furnace, be warming up to 200 DEG C with 3 DEG C/min, be incubated 2h, then be warming up to after 300 DEG C with 3 DEG C/min,
Insulation 8h；Sealing is put in corundum crucible with 500 DEG C of high-temperature roastings 3 hours after filtering oven drying at low temperature after being cooled to room temperature, obtains
The many walls nanotube material of simple substance copper clad, this process need to be protected with vacuum tube furnace.
By mass fraction for Al alloy powder 2% the many walls nanotube material of simple substance copper clad and corresponding mass
7075 Al alloy powders are put into ball milling crucible and are carried out ball milling, whole argon protection, time control in 30min, after by mixed-powder
Pour crucible into, with 10 DEG C/min heating rate to 455 DEG C.Afterwards by crucible move in ultrasonic magnetic agitation stove with 1 DEG C/
Min continues to heat and control its solid rate to open ultrasonic device after 20% scope and work in coordination with lower ultrasonic disperse simultaneously in electromagnetic equipment
Mixing time is controlled in 3min, ultrasonic power 1.0kw, is subsequently poured into corresponding mould and is cooled to room temperature, obtains simple substance copper clad
Many walls nanotube material/7075 aluminium-based semisolid-state blank.
Embodiment 2.
By multi-walled carbon nano-tubes in the ultrasonic pre-dispersed 8h of pure salpeter solution, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleans, is centrifuged to neutrality, then in vacuum drying oven dry for standby.The multi-walled carbon nano-tubes of copper nitrate and above-mentioned drying is made
For raw material, add ultrasonic 50min in straight alcohol；Wherein CNT, copper nitrate and ethanol mol ratio are 1:0.6:127, obtain
Multi-walled carbon nano-tubes suspension；This suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reactor molten long-pending 25%.
Place into heating in reacting furnace, be warming up to 200 DEG C with 5 DEG C/min, be incubated 1h, then be warming up to after 300 DEG C with 3 DEG C/min, insulation
8h；Sealing is put in corundum crucible with 400 DEG C of high-temperature roastings 3 hours after filtering oven drying at low temperature after being cooled to room temperature, obtains simple substance
The many walls nanotube material of copper clad, this process need to be protected with vacuum tube furnace.
By mass fraction for Al alloy powder 3% the many walls nanotube material of simple substance copper clad and 6061 Al alloy powders
End is put into ball milling crucible and is carried out ball milling, whole argon protection, and time control is in 30min.Afterwards by mixed-powder pour into crucible and with
10 DEG C/min heating rate is to 550 DEG C.After proceed in magnetic agitation stove and continue to heat and control its solid rate with 3 DEG C/min
Open ultrasonic device and work in coordination with lower ultrasonic disperse in electromagnetic equipment and mixing time is controlled in 2min, ultrasonic work(after 30% scope
Rate 1.5kw, is subsequently poured into corresponding mould and is cooled to room temperature, obtains many walls nanotube material/6061 aluminium base half of simple substance copper clad
Solid blank.
Embodiment 3.
By multi-walled carbon nano-tubes in the ultrasonic pre-dispersed 8h of pure salpeter solution, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleans, is centrifuged to neutrality, then in vacuum drying oven dry for standby.The multi-walled carbon nano-tubes of copper nitrate and above-mentioned drying is made
For raw material, add ultrasonic 60min in straight alcohol；Wherein multi-walled carbon nano-tubes, copper nitrate and ethanol mol ratio are 1:0.8:127,
Obtain multi-walled carbon nano-tubes suspension；This suspension is imported in hydrothermal reaction kettle, wherein to account for reactor molten long-pending for suspension volume
25%.Place into heating in reacting furnace, be warming up to 200 DEG C with 3 DEG C/min, be incubated 1h, then be warming up to after 300 DEG C with 3 DEG C/min,
Insulation 10h；Sealing is put in corundum crucible with 500 DEG C of high-temperature roastings 3 hours after filtering oven drying at low temperature after being cooled to room temperature, obtains
The many walls nanotube material of simple substance copper clad, this process need to be protected with vacuum tube furnace.
By mass fraction for Al alloy powder 4% the many walls nanotube material of simple substance copper clad and 2024 Al alloy powders
End imports ball milling crucible and carries out ball milling, whole argon protection, and time control is in 30min.Gained mixed powder imports corresponding crucible
With 5 DEG C/min heating rate to 480 DEG C.After proceed in magnetic agitation stove and continue to heat and control its solid phase with 5 DEG C/min
Rate is opened ultrasonic device after 40% scope and is worked in coordination with lower ultrasonic disperse in electromagnetic equipment and mixing time is controlled in 1min, ultrasonic
Power 2.0kw, is subsequently poured into corresponding mould and is cooled to room temperature, obtains many walls nanotube material/2024 aluminium base of simple substance copper clad
Semi-solid blank.
Claims (2)
1. a kind of preparation method of simple substance copper clad multi-walled carbon nano-tubes/aluminum matrix composite semi-solid blank, is characterized in that wrapping
Include following steps:
(1) by multi-walled carbon nano-tubes in the ultrasonic pre-dispersed 6 ~ 8h of pure salpeter solution, temperature is 60 ~ 80 DEG C, after being cooled to room temperature, uses
Deionized water cleans, and is centrifuged to neutrality, then dries in vacuum drying oven, standby；
(2) multi-walled carbon nano-tubes by copper nitrate with through step (1) pretreatment is added in ethanol solution, ultrasonic 40～
60min, obtains carbon nanotube suspension, wherein multi-walled carbon nano-tubes and copper nitrate mol ratio 1:0.4～1:1；
(3) the multi-walled carbon nano-tubes suspension through step (2) is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reaction
Kettle molten long-pending 25%～50%；Place in reacting furnace heating, be warming up to 180～200 DEG C with 1～5 DEG C/s, be incubated 1～2h, then with 1
After～5 DEG C/s is warming up to 300 DEG C, it is incubated 8～12h；Take out, reactor seals air cooling, dried with vacuum drying oven, obtain pre- saw lumber
Material；
(4) put into vacuum tube furnace after putting in corundum crucible through step (3) gained mixing material, 300 ~ 500 DEG C of high temperature roastings
Burn 3 hours, obtain the many walls nanotube material of simple substance copper clad；
(5) the many walls nanotube material of the simple substance copper clad that step (4) is obtained is mixed with Al alloy powder, puts into ball milling crucible and enters
Row ball milling, time control in 30 ~ 60min, the many walls nanotube quality of materials of wherein simple substance copper clad account for Al alloy powder 2% ~
4%, this process is passed through argon and is protected；
(6) step (5) gained mixed-powder is put in crucible, with muffle furnace with 5 ~ 10 DEG C/min heating rate to solid phase
After 10 ~ 20 DEG C below line, proceed in ultrasonic magnetic agitation stove and continue to heat and control its solid rate in 20 ~ 40% with 1 ~ 3 DEG C/min
Scope, ultrasonic and Power Control is in 1.0 ~ 2.0kw, frequency 20khz for indirectly ultrasonic, and stirring at low speed is simultaneously passed through argon protection, surpasses
Sound magnetic agitation time control is in 1 ~ 3min；
(7) step (6) gained semi solid slurry is poured into corresponding mould cooling, obtain simple substance copper clad multi-walled carbon nano-tubes/aluminum
Base composite material semi-solid state blank.
2. preparation method according to claim 1, is characterized in that the hydrothermal reaction kettle liner described in step (3) is polytetrafluoro
Ethylene.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109207781A (en) * | 2018-09-17 | 2019-01-15 | 南昌大学 | A kind of pressing method improving 7075 aluminium alloys |
| CN111286634A (en) * | 2020-02-27 | 2020-06-16 | 南昌航空大学 | Preparation method of cerium oxide-coated graphene oxide aluminum material semi-solid blank |
| US10941464B1 (en) | 2020-06-30 | 2021-03-09 | The Florida International University Board Of Trustees | Metal nanoparticle composites and manufacturing methods thereof by ultrasonic casting |
| CN113373341A (en) * | 2021-06-18 | 2021-09-10 | 苏州第一元素纳米技术有限公司 | Manufacturing process of carbon nano tube reinforced aluminum electric power fitting |
| CN113444906A (en) * | 2021-06-10 | 2021-09-28 | 北京科技大学 | Method for preparing carbon nano tube reinforced light aluminum-based alloy |
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| CN113373341A (en) * | 2021-06-18 | 2021-09-10 | 苏州第一元素纳米技术有限公司 | Manufacturing process of carbon nano tube reinforced aluminum electric power fitting |
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| CN106350695B (en) | 2018-05-04 |
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