CN106244948B - A kind of preparation method for the multi-walled carbon nanotube enhancing magnesium-based composite material for coating elemental copper - Google Patents
A kind of preparation method for the multi-walled carbon nanotube enhancing magnesium-based composite material for coating elemental copper Download PDFInfo
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- CN106244948B CN106244948B CN201610812636.5A CN201610812636A CN106244948B CN 106244948 B CN106244948 B CN 106244948B CN 201610812636 A CN201610812636 A CN 201610812636A CN 106244948 B CN106244948 B CN 106244948B
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- walled carbon
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- C—CHEMISTRY; METALLURGY
- 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
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
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- C—CHEMISTRY; METALLURGY
- 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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- 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
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/04—Light metals
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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 kind of preparation method for the multi-walled carbon nanotube enhancing magnesium-based composite material for coating elemental copper; first prepare the multi-walled carbon nanotube of coating elemental copper; then magnesium alloy powder is imported in the multi-wall carbon nano-tube tube material suspension of coating elemental copper and mixed; 50~100 DEG C of vacuum dryings; ball milling crucible, the lower ball milling of argon gas protection are imported again；50~150MPa is pressed into prefabricated section；It is put into mould, with 10~15 DEG C/min heating rates mould to 10~30 DEG C of subsolidus, then continue to heat with 3~6 DEG C/min again and control its solid rate to obtain the multi-walled carbon nanotube enhancing magnesium-based composite material of coating elemental copper in 70~90% scopes.The present invention has the advantages that simple, safety, low cost are easily operated and controllable.
Description
Technical field
The invention belongs to material to prepare shaping technical field.
Background technology
Magnesium-based composite material has light as a kind of metallic based structures material, and specific strength and specific stiffness are high, good lead
Conductance hot property and damping capacity, the features such as casting character is excellent, it is set to have in metal-base composites bigger
Potential application foreground.But magnesium alloy, equally there is also modulus of elasticity is small, intensity is not high, thermal coefficient of expansion is high, size under high temperature
The shortcomings of stability is poor and wears no resistance so that magnesium alloy has larger limitation as structural material.It is difficult to meet height
Strength structure materials demand.
In recent years, composite strengthening is carried out to magnesium alloy using fiber or particle, the magnesium-based composite material of preparation is due to its height
Specific strength, the advantages that 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
The fields such as its aviation, automobile making, electronic instrument.
CNT is as a kind of tube with a large amount of special excellent properties, such as high intensity, high resiliency, high-ratio surface
Long-pending, heat-resisting, corrosion-resistant, heat conduction and electric conductivity etc., imply CNT has huge application in metal material enhancing research
Prospect.The modulus of CNT is identical with diamond, and theoretical strength has reached 106MPa, it is 100 times of steel, and density is only
For the 1/6 of steel, while it has both extremely excellent toughness and structural stability again, is the preferable choosing as composite enhancing phase
Select.Right carbon pipe is due to its stable SP2Structure, show the wetability of extreme difference simultaneously, CNT is easily rolled into a ball in fusion-casting process
Poly- and wrapping phenomena causes not strong with metallic matrix interfacial bonding property, is unfavorable for the enhancing of composite property.Therefore, how to subtract
Few agglomeration of the CNT in Metal Forming Process, and improve the wetability of itself and matrix to turn into processability excellent
The key of carbon nano-tube reinforced metal-matrix composite material.
It is entitled in publication number CN101966449A：" for a kind of system of multiwall carbon nanotube-supported titanium dioxide catalyst
In Preparation Method ".Solvent heat and hydro-thermal method are combined, adsorb colloid in a solvent, is dried in CNT surface, hydrothermal decomposition its
Colloid, obtain aoxidizing applicator.To reach the purpose of optimization wetability by being modified to CNT surface, right this method step is answered
It is miscellaneous, time length, and simple substance can not be coated in CNT surface, there is certain limitation.
On the other hand, the control to CNT dispersiveness is generally embodied in metal preparation process.At present, stirring is passed through
It is relatively conventional that casting, in-situ synthesis and powder metallurgic method prepare carbon nano-tube reinforced metal-matrix composite material.But this is several
The defects of kind method is also it is clear that for CNT as the flowing of melt is reunited seriously, enhancing distributed mutually is uneven under casting condition
It is even.Powder metallurgy fails effectively to be solved as popular research direction, interface cohesion and fine and close sex chromosome mosaicism.In-situ synthesis
Have that technique is excessively complicated and a short slabs such as process is difficult to control.
In publication number CN103614672A, entitled " preparation method of carbon nanotube enhanced aluminium-based composite material ", adopt
Carbon nano tube enhanced aluminium base is prepared for the conventional powder metallurgical method such as batch mixing, drying, ball milling, cold pressing, sintering and extruding to answer
Condensation material, right interfacial bonding property is poor, more prominent the problems such as material compactness in itself.
In publication number CN103911566A, a kind of entitled " powder metallurgy of carbon nano tube reinforced aluminum alloy composite material
It is more uniform by CNT using powder metallurgy process processing flake aluminum in preparation method ", but conventional powder metallurgical method
The defects of defect does not melt such as, and compactness is not good enough does not solve.
In publication number CN101376932, entitled " CNT enhancing magnesium, aluminum matrix composite and preparation method thereof "
In, reho-forming method is mixed after being heated using powder and prepares CNT enhancing aluminium, magnesium-based composite material.Though densification can be improved
Sex chromosome mosaicism, but CNT easily reunites under rheological condition, and the performance raising to composite is unfavorable.
In publication number CN101376170, entitled " manufacturing equipment of magnesium base-carbon nano tube compound material and its manufacturer
In method ", first carry out magnesium and strengthen the powder mixing of phase particle, heating, recycle a kind of injection device to import the mixture
Extrusion die.Though this method is using thixotroping shaping as innovation, but under this method, to reach mobility effect, magnesium alloy powder melts
Change degree is higher, can still produce and cast similar enhancing phase agglomeration traits so that caused carbon is received in powder mixed process
Mitron dispersion effect weakens.The present invention mainly has following difference with this method：（1）In this method, magnesium alloy powder is hanged by methanol
Floating CNT and ball-milling treatment uniformly mix CNT；（2）In this method, the high solid fraction of mixed-powder is controlled, no
Rheological characteristic can be produced, avoids the multi-walled carbon nanotube under molten condition from reuniting.
The shaping of traditional semisolid die forging experienced half admittedly the preparation of blank, reheat and three procedures of die-forging forming.
Shaped relative to traditional semisolid die forging, short route semi-solid-state shaping has following features：（1）Obtaining semi solid slurry
Afterwards, can be with workpiece once-forming and that acquisition is complex-shaped.（2）Semi-solid-state shaping belongs to near-net forming, easily reaches profile and sets
Meter requires.（3）Semi solid slurry blank has preferable thixotropy, and at low shear rates, slurry behaves like solid-state, without bright
Aobvious mobility, enhancing are mutually not easy to reunite.（4）The viscosity of semi solid slurry blank is high compared to liquid metal and is relatively easy to control,
In whole cavity filling process, it is more steady that semisolid fills type.
The content of the invention
The purpose of the present invention is to propose to a kind of preparation for the multi-walled carbon nanotube enhancing magnesium-based composite material for coating elemental copper
Method.
The present invention is realized by following technology.
A kind of preparation method for the multi-walled carbon nanotube enhancing magnesium-based composite material for coating elemental copper, comprises the following steps.
（1）By multi-walled carbon nanotube, the pre-dispersed 6 ~ 8h of ultrasound, temperature are 60 ~ 80 DEG C in pure salpeter solution, are cooled to room
Wen Hou, cleaned with deionized water, centrifuge to neutrality, then dried in vacuum drying chamber, it is standby.
（2）By copper nitrate and through step（1）The multi-walled carbon nanotube of pretreatment be added in ethanol solution ultrasound 40~
60min, multi-walled carbon nanotube suspension is obtained, wherein CNT and copper nitrate mol ratio are 1:0.4~1:1.
（3）Through step（2）Multi-walled carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for instead
Answer the molten product 25%~50% of kettle.Place into reacting furnace and heat, 180~200 DEG C are warming up to 1~5 DEG C/s, be incubated 1~2h, then with
After 1~5 DEG C/s is warming up to 270 ~ 300 DEG C, 8~12h is incubated；Take out, air cooling, filtering drying, obtain coating more walls of elemental copper
Carbon nano-tube material.
（4）The multi-wall carbon nano-tube tube material for coating elemental copper is added into low power ultrasonic vibration≤30min in methanol, applied
Cover the multi-wall carbon nano-tube tube material suspension of elemental copper.
（5）Magnesium alloy powder is added to stir in the multi-wall carbon nano-tube tube material suspension of coating elemental copper and mixed
Batch mixing, and in 50 ~ 100 DEG C of vacuum dryings, wherein the mass percent of the multi-wall carbon nano-tube tube material of coating elemental copper closes for magnesium
The 1% ~ 4% of bronze.
（6）Step（5）Obtained batch mixing imports ball milling crucible and carries out ball milling, and whole process is passed through argon gas in the mechanical milling process
Protected.
（7）Step（6）Gained mixed-powder is put into 50 ~ 150MPa in mould and is pressed into prefabricated section.
（8）Step（7）Gained prefabricated section is put into corresponding mold groove, should with 8 ~ 13 DEG C/min heating rates
Mould is to 10 ~ 30 DEG C of subsolidus.Continue to heat with 3 ~ 6 DEG C/min and control its solid rate in 70 ~ 90% scopes.
（9）Step（8）Gained moulding mixture carries out die-forging forming, and pressure head is controlled after 1 ~ 100mm/s speed, 1 ~ 3min of pressurize
It is cooled to the multi-walled carbon nanotube enhancing magnesium-based composite material drip molding that room temperature obtains coating elemental copper.
The present invention has following uniqueness：（1）Solution uses ethanol rather than water, participates in reaction in itself and increases volatilization
Property, pressure is bigger, beneficial to the surface tension of reduction solution.（2）Usual nitric acid metal carbonyl compound in a heated condition can only
Oxide is decomposed into, and the present invention can generate copper simple substance.（3）The easy and effective operation difficulty of this method is low.（4）This method is not required to hold high
Your instrument, reaction temperature is relatively low, and danger coefficient is low.（5）Multi-walled carbon nanotube is combined under the conditions of magnesium alloy semi solid state with matrix,
With more preferable interface simultaneously, the reunion of multi-walled carbon nanotube under the conditions of founding is avoided.
The present invention is to overcome the system of multi-walled carbon nanotube magnesium-based composite material using short route semisolid contour forming method
Standby defect, short route semisolid contour forming is the combination of semi-solid rheological and contour forging technique.Its microstructure of semisolid, which includes, uniformly divides
Dissipate in the spheric grain of remaining liquid phase, and there is high solid fraction.It is molded under this condition, strengthens the probability mutually reunited and reduce, together
When ensure semisolid die forging shaping advantage when, significantly shorten forming period.
Brief description of the drawings
Accompanying drawing 1 is the multi-walled carbon nanotube microscopic structure picture of coating elemental copper prepared by embodiment 3.
Embodiment
The present invention will be described further by following examples.
Embodiment 1.
By multi-walled carbon nanotube in the pure salpeter solution pre-dispersed 8h of ultrasound, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleaning, centrifuge to neutrality, be then dried for standby in vacuum drying chamber.Using copper nitrate and the CNT of above-mentioned drying as
Raw material, add ultrasonic 40min in ethanol solution；Wherein CNT, copper nitrate and ethanol mol ratio are 1:0.4:127, obtain
Multi-walled carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product 25% of reactor.
Place into reacting furnace and heat, be warming up to 200 DEG C with 5 DEG C/s, be incubated 1h, then after being warming up to 270 DEG C with 5 DEG C/s, be incubated 8h；
Take out, air cooling, filtering drying, obtain coating the multi-wall carbon nano-tube tube material of elemental copper.
Mass percent is put into low power in methanol for the multi-walled carbon nanotube of 2% coating elemental copper of magnesium alloy powder to surpass
Acoustic shock swings to obtain the multi-walled carbon nanotube suspension of coating elemental copper, time control 20min.The AZ61 powder of corresponding mass is put
Enter suspension to obtain mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 50MPa in mould and is pressed into
Block, gained prefabricated section be put into corresponding in mold groove, it is heated with the 10 DEG C/min heating rates mould to 500 DEG C
Argon gas protection is passed through in journey.Continue to heat with 3 DEG C/min and control its solid rate in 90% or so it is rear carry out die-forging forming processing,
With 10mm/s pressure head speed, the dwell time to be cooled to room temperature after 1min, obtains coating multi-walled carbon nanotube/AZ61 of elemental copper
Magnesium-based composite material drip molding.
Embodiment 2.
By multi-walled carbon nanotube in the pure salpeter solution pre-dispersed 8h of ultrasound, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleaning, centrifuge to neutrality, be then dried for standby in vacuum drying chamber.Using copper nitrate and the CNT of above-mentioned drying as
Raw material, add ultrasonic 40min in ethanol solution；Wherein multi-walled carbon nanotube, copper nitrate and ethanol mol ratio are 1:0.7:127,
Obtain multi-walled carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product of reactor
30%.Place into reacting furnace and heat, be warming up to 200 DEG C with 5 DEG C/s, be incubated 1h, then after being warming up to 280 DEG C with 5 DEG C/s, insulation
10h；Take out, air cooling, filtering drying, obtain coating the multi-wall carbon nano-tube tube material of elemental copper.
Mass percent is put into low power in methanol for the multi-walled carbon nanotube of 3% coating elemental copper of magnesium alloy powder to surpass
Acoustic shock swings to obtain the multi-walled carbon nanotube suspension of coating elemental copper, time control 20min.By the AZ91D magnesium of corresponding mass
Alloyed powder imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.It is cold that gained mixed-powder is put into 100MPa in mould
Briquet is pressed, gained prefabricated section is put into corresponding mold groove, with 10 DEG C/min heating rates mould to 450
DEG C, argon gas or vacuum protection in heating process.Continue to heat with 5 DEG C/min and control its solid rate in 80% or so rear carry out mould
Forging molding processing, with 50mm/s pressure head speed, the dwell time to be cooled to room temperature after 2min, obtains coating more wall carbon of elemental copper
Nanotube/AZ61D magnesium-based composite material drip moldings.
Embodiment 3.
By multi-walled carbon nanotube in the pure salpeter solution pre-dispersed 8h of ultrasound, temperature is 60 DEG C, after being cooled to room temperature, spend from
Sub- water cleaning, centrifuge to neutrality, be then dried for standby in vacuum drying chamber.With copper nitrate and the multi-walled carbon nanotube of above-mentioned drying
As raw material, ultrasonic 60min in ethanol solution is added；Wherein multi-walled carbon nanotube, copper nitrate and ethanol mol ratio are 1:1:
127, obtain multi-walled carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reactor
Molten product 40%.Place into reacting furnace and heat, be warming up to 200 DEG C with 5 DEG C/s, be incubated 1h, then after being warming up to 300 DEG C with 5 DEG C/s,
It is incubated 12h；Take out, air cooling, filtering drying, obtain coating the multi-wall carbon nano-tube tube material of elemental copper.
Mass percent is put into low power in methanol for the multi-walled carbon nanotube of 2% coating elemental copper of magnesium alloy powder to surpass
Acoustic shock swings to obtain the multi-walled carbon nanotube suspension of coating elemental copper, time control 20min.The AZ31 magnesium of corresponding mass is closed
Bronze imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 150MPa in mould and is cold-pressed
Briquet, gained prefabricated section is put into corresponding mold groove, with the 10 DEG C/min heating rates mould to 520 DEG C,
Argon gas or vacuum protection in heating process.Continue to heat with 5 DEG C/min and control its solid rate in 70% or so it is rear carry out die forging into
Type processing, with 70mm/s pressure head speed, the dwell time to be cooled to room temperature after 3min, obtains coating the multi-wall carbon nano-tube of elemental copper
Pipe/AZ31 magnesium-based composite material drip moldings.
Claims (1)
- A kind of 1. preparation method for the multi-walled carbon nanotube enhancing magnesium-based composite material for coating elemental copper, it is characterized in that including following Step：（1）By multi-walled carbon nanotube in pure salpeter solution the pre-dispersed 6 ~ 8h of ultrasound, temperature is 60 ~ 80 DEG C, after being cooled to room temperature, Cleaned with deionized water, centrifuge to neutrality, then dried in vacuum drying chamber, it is standby；（2）By copper nitrate and through step（1）The multi-walled carbon nanotube of pretreatment be added in ethanol solution ultrasound 40~ 60min, multi-walled carbon nanotube suspension is obtained, wherein CNT and copper nitrate mol ratio are 1:0.4~1:1；（3）Through step（2）Multi-walled carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for reactor Volume 25%~50%；Place into reacting furnace and heat, be warming up to 180~200 DEG C with 1~5 DEG C/s, be incubated 1~2h, then with 1~5 DEG C/after s is warming up to 270 ~ 300 DEG C, it is incubated 8~12h；Take out, air cooling, filtering drying, the more wall carbon for obtaining coating elemental copper are received Nanotube material；（4）The multi-wall carbon nano-tube tube material for coating elemental copper is added into low power ultrasonic vibration≤30min in methanol, it is single to obtain coating The multi-wall carbon nano-tube tube material suspension of matter copper；（5）Magnesium alloy powder is added into stirring in the multi-wall carbon nano-tube tube material suspension of coating elemental copper to obtain mixing batch mixing, And in 50 ~ 100 DEG C of vacuum dryings, wherein the mass percent of the multi-wall carbon nano-tube tube material of coating elemental copper is magnesium alloy powder 1% ~ 4%；（6）Step（5）Obtained batch mixing imports ball milling crucible and carries out ball milling, and whole process is passed through argon gas progress in the mechanical milling process Protection；（7）Step（6）Gained mixed-powder is put into 50 ~ 150MPa in mould and is pressed into prefabricated section；（8）Step（7）Gained prefabricated section is put into corresponding mold groove, with 8 ~ 13 DEG C/min heating rates mould To 10 ~ 30 DEG C of subsolidus；Continue to heat with 3 ~ 6 DEG C/min and control its solid rate in 70 ~ 90% scopes；（9）Step（8）Gained moulding mixture carries out die-forging forming, and pressure head control cools down after 1 ~ 100mm/s speed, 1 ~ 3min of pressurize Obtaining coating the multi-walled carbon nanotube of elemental copper to room temperature strengthens magnesium-based composite material molding part.
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| JP2007016262A (en) * | 2005-07-06 | 2007-01-25 | Nissan Motor Co Ltd | Carbon nanotube-containing composite material, and method for producing the same |
| CN101376932B (en) * | 2007-08-31 | 2010-11-10 | 清华大学 | Preparation and preparing apparatus for magnesium-based composite material |
| TWI346711B (en) * | 2007-12-14 | 2011-08-11 | Hon Hai Prec Ind Co Ltd | Method of making magnesium matrix nanotube composite material |
| JP4990251B2 (en) * | 2008-09-19 | 2012-08-01 | 日精樹脂工業株式会社 | Composite method of carbon nanomaterial and magnesium-based alloy |
| CN103014399B (en) * | 2012-12-31 | 2014-07-30 | 哈尔滨工业大学 | Preparation method of enhanced magnesium-based composite material of carbon nanotubes |
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