CN106367630B - A kind of preparation method for the multi-walled carbon nanotube reinforced aluminum matrix composites for coating elemental copper - Google Patents
A kind of preparation method for the multi-walled carbon nanotube reinforced aluminum matrix composites for coating elemental copper Download PDFInfo
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- CN106367630B CN106367630B CN201610812637.XA CN201610812637A CN106367630B CN 106367630 B CN106367630 B CN 106367630B CN 201610812637 A CN201610812637 A CN 201610812637A CN 106367630 B CN106367630 B CN 106367630B
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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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
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- C22C2026/002—Carbon nanotubes
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Abstract
A kind of preparation method for the multi-walled carbon nanotube reinforced aluminum matrix composites for coating elemental copper; first prepare the multi-walled carbon nanotube of coating elemental copper; then Al alloy powder is imported in the multi-wall carbon nano-tube tube material suspension of coating elemental copper and obtains mixture; 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 10~20 DEG C of subsolidus, then continue to heat with 5~8 DEG C/min again and control its solid rate to obtain the multi-walled carbon nanotube reinforced aluminum matrix composites 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 technical field of material.
Background technology
In recent years, fiber reinforced aluminum matrix composites are due to its high specific strength, good electrical and thermal conductivity performance and low-heat
The advantages that coefficient of expansion, attracted very big concern and be widely used in the fields such as space flight and aviation, automobile making, electronic instrument.
Carbon nanotubes is the tube formed by the curling of graphite hexagonal network, has unique hollow nano structure, envelope
The topology configuration and helical structure closed so that with a large amount of special excellent properties, as high intensity, high resiliency, high-specific surface area,
Heat-resisting, corrosion-resistant, heat conduction and electric conductivity etc., imply carbon nanotubes has huge application space in materials application research.Carbon
The modulus of nanotube is identical with diamond, and theoretical strength has reached 106Megapascal, is 100 times of steel, and density is only steel
1/6, while it has both extremely excellent toughness and structural stability again, is the ideal chose as composite material enhancing phase.Right CNT's
Defect is also apparent.Carbon pipe is due to its stable SP2Structure, shows very poor wetability at the same time, carbon nanotubes 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, agglomeration of the carbon nanotubes in Metal Forming Process how is reduced, and improve itself and the wetability of matrix to become
The key of the excellent carbon nano-tube reinforced metal-matrix composite material of processability.
Carbon nanotubes, which improves wetability method, at present overlay coating etc., and such as chemical nickel plating, this method mainly will complete base
The carbon nanotubes of change is through sensitization plays, after activation, is put into plating in chemical plating fluid, can be in carbon nano tube surface with the progress of reaction
Continuous, uniform coating is obtained, but it is expensive, and toxic reagent is commonly used, not environmentally and production cost is high, is not suitable for big rule
Mould produces.Sol method is also popular research coating direction, adds organic compound in the solution and stirs, reaction a period of time,
Then carbon nanotubes is added, acid group metallic compound is added and is kept stirring state until generation colloidal sol, sky is exposed to by this colloid
Aging in gas, after a few days dries product grind into powder, is heat-treated in last certain temperature inert gas flow and obtains for a period of time
To nano-complex particle.But the proportioning difficulty of amount is big, and the reaction time is long.
It is entitled in 101966449 A of publication CN：" for a kind of carbon multi-wall nano tube loaded Titanium Dioxide
In the preparation method of agent ".Solvent heat and hydro-thermal method are combined, adsorb colloid in a solvent, it is dry in CNT surface, hydro-thermal
Its colloid is decomposed, obtains oxidation applicator.Right this method step is complicated, time length, and cannot coat simple substance in CNT surface,
With certain limitation.
On the other hand, the control to carbon nanotubes dispersiveness is usually embodied in made of metal for during.At present, stirring is passed through
It is relatively conventional that casting, in-situ synthesis and powder metallurgic method prepare the strong aluminum matrix composite of carbon nanotubes.But these types side
The defects of method is also that enhancing distributed mutually is uneven, powder it is clear that CNT is as the flowing of melt is reunited seriously under casting condition
Last metallurgy is popular research direction, but interface cohesion and fine and close sex chromosome mosaicism fail effectively to be solved.In-situ synthesis exists
The short slabs such as technique is excessively complicated and 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
The problems such as condensation material, right interfacial bonding property is poor, material compactness in itself is more prominent.
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 " carbon nanotubes enhancing magnesium, aluminum matrix composite and preparation method thereof "
In, reho-forming method is mixed after being heated using powder and prepares carbon nanotubes 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 material is unfavorable.
Therefore, prepared in conclusion still lacking a kind of cost-effective carbon nanotube enhanced aluminium-based composite material at present
Technology.
Compared with traditional material technology of preparing, short route semisolid die forging is formed with following features：（1）Semi-solid forming
Temperature is compared to the moulding extruding of powder metallurgy more than solidus, and interfacial bonding property is more preferable.（2）Semi-solid-state shaping belongs to
Near-net forming, easily reaches configuration design requirement.（3）Semi solid slurry blank has preferable thixotropy, in low shear rate
Under, slurry behaves like solid-state, and without obvious mobility, enhancing is mutually not easy to reunite.（4）The viscosity of semi solid slurry blank is compared
In liquid metal height and it 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 reinforced aluminum matrix composites for coating elemental copper
Method.
The present invention is achieved by the following technical solutions.
A kind of preparation method for the multi-walled carbon nanotube reinforced aluminum matrix composites 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, is cleaned with deionized water, is centrifuged to neutrality, is then dried in vacuum drying chamber, spare.
（2）By copper nitrate and through step（1）The multi-walled carbon nanotube of pretreatment is added in ethanol solution, and ultrasound 40~
60min, obtains multi-walled carbon nanotube suspension, wherein multi-walled carbon nanotube and copper nitrate molar ratio 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, keep the temperature 1~2h, then with
After 1~5 DEG C/s is warming up to 260 DEG C, 8~12h is kept the temperature；Take out, air-cooled, filtering drying, the multi wall carbon for obtaining coating elemental copper is 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, is applied
Cover the multi-wall carbon nano-tube tube material suspension of elemental copper.
（5）Al alloy powder is imported in the multi-wall carbon nano-tube tube material suspension of coating elemental copper and obtains mixture, and
50 ~ 100 DEG C of vacuum dryings.Wherein, coat the mass percent of the multi-wall carbon nano-tube tube material of elemental copper for Al alloy powder 1% ~
4%.
（6）Step（5）Obtained mixture imports ball milling crucible and carries out ball milling, be passed through in the mechanical milling process argon gas into
Row protection.
（7）Step（6）Gained mixed-powder is put into mould, and 50 ~ 150MPa is pressed into prefabricated section.
（8）Step（7）Gained prefabricated section is put into corresponding mold groove, with 10 ~ 15 DEG C/min heating rates
Then the mould continues to heat and controls its solid rate in 70 ~ 90% models with 5 ~ 8 DEG C/min again to 10 ~ 20 DEG C of subsolidus
Enclose.
（9）Step（8）Gained moulding mixture carries out die-forging forming, and pressure head is controlled in 1 ~ 100mm/s speed, 1 ~ 4min of pressurize
Postcooling obtains the multi-walled carbon nanotube reinforced aluminum matrix composites drip molding of coating elemental copper to room temperature.
Step of the present invention（3）The hydrothermal reaction kettle liner is polytetrafluoroethylene (PTFE).
The present invention is shaped using short route semisolid die forging to overcome the preparation defect of carbon nanotubes aluminum matrix composite.Half
A kind of material forming techniques of the solid die forging into the combination of form semi-solid rheological and contour forging technique.This short route high solid fraction
Semisolid die forging shape, it is not necessary to prepare blank and reheat step, after semi solid slurry is obtained, can it is once-forming and
Complex-shaped workpiece is obtained, the reunion of carbon nanotubes, agglomerating phenomenon can be reduced.
The present invention has following uniqueness：（1）Solution uses ethanol rather than water, participates in reaction in itself and increases volatilization
Property, pressure bigger is 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）This method is easy and effective to be suitable for batch production.（4）This method is not
Expensive instrument is needed, reaction temperature is relatively low, and danger coefficient is low.（5）Multi-walled carbon nanotube under the conditions of aluminium alloy semi-solid with matrix
With reference to, have more preferable interface at the same time, avoid the reunion of multi-walled carbon nanotube under the conditions of founding.
Brief description of the drawings
Fig. 1 is coating multi-walled carbon nanotube microscopic structure picture prepared by embodiment 3.
Embodiment
The present invention will be described further by following embodiments.
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, is then dried for standby in vacuum drying chamber.With copper nitrate and the multi-walled carbon nanotube of appeal drying
As raw material, ultrasound 40min in ethanol solution is added；Wherein multi-walled carbon nanotube, copper nitrate and ethanol molar 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 reaction kettle
Molten product 25%.Place into reacting furnace and heat, be warming up to 200 DEG C with 5 DEG C/s, keep the temperature 1h, then after being warming up to 300 DEG C with 5 DEG C/s,
Keep the temperature 8h；Take out, air-cooled, filtering drying, obtain the multi-wall carbon nano-tube tube material of coating elemental copper.
Mass percent is put into low power in methanol for the multi-walled carbon nanotube of 2% coating elemental copper of Al alloy powder to surpass
Acoustic shock swings to obtain the multi-walled carbon nanotube suspension of coating elemental copper, time control 20min.7075 aluminium of corresponding mass are closed
Bronze imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 50MPa in mould and is cold-pressed
Briquet, gained prefabricated section are put into corresponding mold groove, with the 10 DEG C/min heating rates mould to 455 DEG C.
Continue to heat with 5 DEG C/min and control its solid rate in 90% or so it is rear carry out die-forging forming processing, with 20mm/s pressure head speed,
Dwell time is 1min postcoolings to room temperature, obtains the aluminum matrix composite of the multi-walled carbon nanotube of coating elemental copper/7075.
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, is then dried for standby in vacuum drying chamber.With copper nitrate and the multi-walled carbon nanotube of appeal drying
As raw material, ultrasound 40min in ethanol solution is added；Wherein multi-walled carbon nanotube, copper nitrate and ethanol molar 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 reaction kettle
Molten product 30%.Place into reacting furnace and heat, be warming up to 200 DEG C with 50 DEG C/s, keep the temperature 1h, then 260 DEG C are warming up to 50 DEG C/s
Afterwards, 10h is kept the temperature；Take out, air-cooled, filtering drying, obtain the multi-wall carbon nano-tube tube material of coating elemental copper.
Mass percent is put into low power in methanol for the multi-walled carbon nanotube of 3% coating elemental copper of Al alloy powder to surpass
Acoustic shock swings to obtain the multi-walled carbon nanotube suspension of coating elemental copper, time control 20min.6061 aluminium of corresponding mass are closed
Bronze imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 100MPa in mould and is cold-pressed
Briquet, gained prefabricated section are put into corresponding mold groove, with the 10 DEG C/min heating rates mould to 550 DEG C.
Continue to heat with 5 DEG C/min and control its solid rate in 80% or so it is rear carry out die-forging forming processing, with 50mm/s pressure head speed,
Dwell time is 2min postcoolings to room temperature, obtains the aluminum matrix composite of the multi-walled carbon nanotube of coating elemental copper/6061.
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, is then dried for standby in vacuum drying chamber.With copper nitrate and the multi-walled carbon nanotube of appeal drying
As raw material, ultrasound 60min in ethanol solution is added；Wherein multi-walled carbon nanotube, copper nitrate and ethanol molar ratio are 1:1:
127, obtain multi-walled carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reaction kettle
Molten product 40%.Place into reacting furnace and heat, be warming up to 200 DEG C with 5 DEG C/s, keep the temperature 1h, then after being warming up to 280 DEG C with 5 DEG C/s,
Keep the temperature 12h；Take out, air-cooled, filtering drying, obtain the multi-wall carbon nano-tube tube material of coating elemental copper.
Mass percent is put into low power in methanol for the multi-walled carbon nanotube of 3% coating elemental copper of Al alloy powder to surpass
Acoustic shock swings to obtain the multi-walled carbon nanotube suspension of coating elemental copper, time control 20min.2024 aluminium of corresponding mass are 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 are put into corresponding mold groove, with the 10 DEG C/min heating rates mould to 480 DEG C.
Continue to heat with 5 DEG C/min and control its solid rate in 70% or so it is rear carry out die-forging forming processing, with 70mm/s pressure head speed,
Dwell time is 3min postcoolings to room temperature, obtains the aluminum matrix composite of the multi-walled carbon nanotube of coating elemental copper/2024.
Claims (2)
- A kind of 1. method for the multi-walled carbon nanotube reinforced aluminum matrix composites for coating elemental copper, it is characterized in that including following step Suddenly：（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 spare；（2）By copper nitrate and through step（1）The multi-walled carbon nanotube of pretreatment is added in ethanol solution, 40~60min of ultrasound, Obtain multi-walled carbon nanotube suspension, wherein multi-walled carbon nanotube and copper nitrate molar ratio 1:0.4~1:1；（3）Through step（2）Multi-walled carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for reaction kettle Volume 25%~50%；Place into reacting furnace and heat, be warming up to 180~200 DEG C with 1~5 DEG C/s, keep the temperature 1~2h, then with 1~5 DEG C/after s is warming up to 260 DEG C, keep the temperature 8~12h；Take out, air-cooled, filtering drying, obtain the multi-walled carbon nanotube of coating elemental copper 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）Al alloy powder is imported in the multi-wall carbon nano-tube tube material suspension of coating elemental copper and obtains mixing batch mixing, and 50 ~ 100 DEG C of vacuum dryings；Wherein, coat the mass percent of the multi-wall carbon nano-tube tube material of elemental copper for Al alloy powder 1% ~ 4%；（6）Step（5）Obtained batch mixing imports ball milling crucible and carries out ball milling, and being passed through argon gas in the mechanical milling process is protected Shield；（7）Step（6）Gained mixed-powder is put into mould, and 50 ~ 150MPa is pressed into prefabricated section；（8）Step（7）Gained prefabricated section is put into corresponding mold groove, with 10 ~ 15 DEG C/min heating rates mould Then tool continues to heat and controls its solid rate in 70 ~ 90% scopes with 5 ~ 8 DEG C/min again to 10 ~ 20 DEG C of subsolidus；（9）Step（8）Gained moulding mixture carries out die-forging forming, and pressure head control is cold after 1 ~ 100mm/s speed, 1 ~ 4min of pressurize But to room temperature, the multi-walled carbon nanotube reinforced aluminum matrix composites of coating elemental copper are obtained.
- 2. according to the method described in claim 1, it is characterized in that step（3）The hydrothermal reaction kettle liner is polytetrafluoroethyl-ne Alkene.
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| CN114890408B (en) * | 2022-05-12 | 2023-08-22 | 湖南湘投轻材科技股份有限公司 | Preparation method of carbon nano tube with controllable size distribution and preparation method of carbon nano tube reinforced aluminum matrix composite material |
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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 |
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