CN106399880B - A kind of preparation method of coating alumina whisker carbon nanotube enhanced aluminium-based composite material - Google Patents
A kind of preparation method of coating alumina whisker carbon nanotube enhanced aluminium-based composite material Download PDFInfo
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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
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- C—CHEMISTRY; METALLURGY
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- 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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- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
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Abstract
A kind of preparation method of the whisker carbon nanotube enhanced aluminium-based composite material of coating alumina; first prepare the whisker carbon nanotubes of coating alumina; then Al alloy powder is imported in the whisker carbon nanotube suspension of coating alumina and obtains batch mixing; 50~100 DEG C of vacuum dryings; ball milling crucible, the lower ball milling of argon gas protection are imported again；60~150MPa is pressed into prefabricated section；It is put into mold, the mold is heated to 10~20 DEG C of subsolidus with 5~10 DEG C/min rates of heat addition, then continue to heat with 1~5 DEG C/min again and its solid rate is controlled to obtain the multi-walled carbon nanotube reinforced aluminum matrix composites of coating elemental copper in 70~90% scopes.The present invention has many advantages, such as that simple, safety, low cost are easily operated and controllable.
Description
Technical field
The invention belongs to material preparation forming technique fields.
Background technology
Aluminium alloy is most widely used one kind structural metallic materials in industry, has light, specific strength is high, plasticity is good etc.
Feature can be processed into various section bars.It is widely used, and is largely used in the industries such as Aeronautics and Astronautics, automobile, ship.Industry warp
Today of the rapid development of Ji, increasing to the demand of Al-alloy parts, people are consequently increased the performance requirement of aluminium alloy.
In recent years, composite strengthening is carried out to magnesium alloy using fiber or particle, the aluminum matrix composite 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.
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 as to 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 material application study.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 simultaneously, and carbon nanotubes is in founding
Easily reunite in the process and wrapping phenomena causes not strong with metallic matrix interfacial bonding property, be unfavorable for the increasing of composite property
By force.Therefore, how reducing agglomeration of the carbon nanotubes in Metal Forming Process and improving itself and the wetability of matrix becomes
The key of the excellent carbon nano-tube reinforced metal-matrix composite material of processability.
For crystal whisker-shaped carbon nanotube as a kind of new structure carbon nanotubes, being compared to original carbon nanotubes has surface more
Add smooth, highly polished, the features such as diameter change is little and curvature is low, outer diameter is distributed between 50~200nm, length
It is distributed between 2~20 μm.Mixed and disorderly degree of aggregation is low, can promote the dispersing technology of carbon nanotubes to a certain extent, be received for carbon
The industrialization of mitron uses and provides greatly possibility.
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 in organic compound in the solution and stirs, reaction a period of time,
Then carbon nanotubes is added in, acid group metallic compound is added in 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, and the time is long, and cannot coat simple substance in CNT surface,
With certain limitation.
On the other hand, made of metal is usually embodied in the control of carbon nanotubes dispersiveness 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.However these types side
The defects of method is also it is clear that CNT is as the flowing of melt is reunited seriously under casting condition, and enhancing distributed mutually is uneven, powder
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 metallurgicals 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 it is unfavorable that the performance of composite material is improved.
Therefore, prepared in conclusion still lacking a kind of cost-effective carbon nanotube enhanced aluminium-based composite material at present
Forming technique.
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 apparent mobility, enhancing is mutually not easy to reunite.（4）The viscosity of semi solid slurry blank is compared
It in liquid metal height and is relatively easy to control, in entire 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 preparations of the whisker carbon nanotube enhanced aluminium-based composite material of coating alumina
Method.
The present invention is achieved by the following technical solutions.
A kind of preparation method of the whisker carbon nanotube enhanced aluminium-based composite material of coating alumina of the present invention, bag
Include following steps：
（1）By whisker carbon nanotubes in the pure salpeter solution pre-dispersed 6 ~ 8h of ultrasound, temperature is 60 ~ 80 DEG C, is cooled to room temperature
Afterwards, cleaned with deionized water, centrifuge to neutrality, then dried in vacuum drying chamber, it is spare；
（2）By aluminum nitrate and through step（1）The whisker carbon nanotubes of pretreatment be added in methanol solution ultrasound 40~
60min obtains whisker carbon nanotube suspension, wherein whisker carbon nanotubes and nitric acid al mole ratio 1:0.4~1:1；
（3）Through step（2）Whisker carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for instead
Answer the molten product 25%~40% of kettle.It places into reacting furnace and heats, 100~120 DEG C are warming up to 1~5 DEG C/min, keep the temperature 1~2h, then
After being warming up to 150 DEG C with 1~3 DEG C/min, 8~12h is kept the temperature；Low temperature drying is filtered after being cooled to room temperature with 5 ~ 10 DEG C/min；
（4）Through step（3）Gained mixing material is put into corundum crucible, whole when 480 ~ 700 DEG C of high-temperature roastings 3 are small
Argon gas protection is imported, obtains the whisker carbon nano-tube material of coating alumina；
（5）The whisker carbon nano-tube material of coating alumina is put into low power ultrasonic vibration≤30min in methanol, is obtained
The whisker carbon nanotube suspension of coating alumina；
（5）Al alloy powder is imported in suspension and is stirred, obtains mixture, and in 50 ~ 100 DEG C of vacuum dryings.Wherein apply
The whisker carbon nanotubes for covering aluminium oxide accounts for the 1% ~ 4% of aluminium alloy gross mass.
（6）Step（5）Obtained mixture is put into ball milling crucible and carries out ball milling, and argon gas is passed through in the mechanical milling process
It is protected；
（7）Step（6）Gained mixed-powder is put into 60 ~ 150MPa in mold and is pressed into prefabricated section；
（8）Step（7）Gained prefabricated section is put into corresponding mold groove, is heated with 5 ~ 10 DEG C/min rates of heat addition
To 10 ~ 20 DEG C of subsolidus, 1 ~ 5 DEG C/min continues to heat and controls its solid rate in 70 ~ 90% scopes the mold；
（9）Step（8）Gained moulding mixture carries out die-forging forming, pressure head control in 20 ~ 130mm/s rates, pressurize 5 ~
10min postcoolings to room temperature obtains the whisker carbon nanotube enhanced aluminium-based composite material drip molding of coating alumina.
Step of the present invention（3）The hydrothermal reaction kettle liner is polytetrafluoroethylene (PTFE).
The present invention shapes to overcome the preparation defect of CNT aluminum matrix composites using short route semisolid die forging.Semisolid
Die-forging forming is a kind of material forming techniques of the combination of semi-solid rheological and contour forging technique.This short route high solid fraction half is solid
State die-forging forming need not prepare blank and reheat step, can once-forming and acquisition after semi solid slurry is obtained
Complex-shaped workpiece can reduce the reunion of CNT, agglomerating phenomenon.
The present invention has following uniqueness：（1）Solution uses methanol rather than water, and volatility is larger under heating condition, pressure
Strong bigger is beneficial to the surface tension of reduction solution.（2）The oxidation decomposed in a heated condition using nitric acid metal carbonyl compound
Object is deposited directly on whisker.（3）The simple and effective operation difficulty of this method is low.（4）This method is not required to expensive instrument, reaction temperature
Relatively low, danger coefficient is low.（5）Whisker carbon nanotubes is combined under the conditions of aluminium alloy semi-solid with matrix, has better interface
Meanwhile avoid the reunion of carbon nanotubes under the conditions of founding.（6）It is tried using more straight and short carbon nano-tube material
It tests, further reduces the probability that carbon nanotubes is reunited.
Description of the drawings
Attached drawing 1 is that whisker carbon nanotubes displaing micro picture is used in the present invention.
Attached drawing 2 is original multi-walled carbon nanotube microscopic structure picture.
Specific embodiment
The present invention will be described further by following embodiment.
Embodiment 1.
By whisker carbon nanotubes 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 is centrifuged to neutrality, is then dried for standby in vacuum drying chamber.With aluminum nitrate and the whisker carbon nanotubes of above-mentioned drying
As raw material, ultrasound 40min in methanol solution is added in；Wherein whisker carbon nanotubes, aluminum nitrate and methanol molar ratio are 1:0.4:
182, obtain whisker carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reaction kettle
Molten product 25%.It places into reacting furnace and heats, be warming up to 100 DEG C with 5 DEG C/min, keep the temperature 1h, then 150 DEG C are warming up to 3 DEG C/min
Afterwards, 8h is kept the temperature；It is put into after being cooled to room temperature with 5 DEG C/min after filtering low temperature drying in corundum crucible small with 500 DEG C of high-temperature roastings 3
When, the whisker carbon nano-tube material of coating alumina is obtained, the process is whole to import argon gas protection.
Mass percent is put into low power in methanol for the whisker carbon nanotubes of 2% coating alumina of Al alloy powder to surpass
Acoustic shock swings to obtain the whisker carbon nanometer suspension of coating alumina, time control 20min.By 7075 aluminium alloys of corresponding mass
Powder imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 150MPa cold pressings pressure in mold
Block is made, gained prefabricated section is put into corresponding mold groove, and the mold is heated to 455 DEG C with the 10 DEG C/min rates of heat addition.With 1
DEG C/min continues to heat and controls its solid rate after 90% scope with 20mm/s pressure head rates, the dwell time is 9min postcoolings
To room temperature, the aluminum matrix composite drip molding of the whisker carbon nanotubes of coating alumina/7075 is obtained.
Embodiment 2.
By whisker carbon nanotubes 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 is centrifuged to neutrality, is then dried for standby in vacuum drying chamber.With aluminum nitrate and the whisker carbon nanotubes of above-mentioned drying
As raw material, ultrasound 40min in methanol solution is added in；Wherein carbon nanotubes, aluminum nitrate and methanol molar ratio are 1:0.7:182,
Obtain whisker carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for the molten product of reaction kettle
30%.It places into reacting furnace and heats, be warming up to 120 DEG C with 3 DEG C/min, keep the temperature 1h, then after being warming up to 150 DEG C with 1 DEG C/min,
Keep the temperature 10h；It is put into after being cooled to room temperature with 7 DEG C/min after filtering low temperature drying in corundum crucible small with 600 DEG C of high-temperature roastings 3
When, the whisker carbon nano-tube material of coating alumina is obtained, the process is whole to import argon gas protection.
Mass fraction is put into low power ultrasound in methanol for the whisker carbon nanotubes of 3% coating alumina of Al alloy powder
Concussion obtains the whisker carbon nanotube suspension of coating alumina, time control 20min.By 6061 aluminium alloys of corresponding mass
Powder imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 100MPa cold pressings pressure in mold
Block is made, gained prefabricated section is put into corresponding mold groove, and the mold is heated to 550 DEG C with the 10 DEG C/min rates of heat addition.With 3
DEG C/min continue to heat and control its solid rate in 80% or so it is rear carry out die-forging forming processing, with 50mm/s pressure head rates, pressurize
Time is 7min postcoolings to room temperature, obtains the aluminum matrix composite drip molding of the whisker carbon nanotubes of coating alumina/6061.
Embodiment 3.
By whisker carbon nanotubes 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 is centrifuged to neutrality, is then dried for standby in vacuum drying chamber.With aluminum nitrate and the whisker carbon nanotubes of above-mentioned drying
As raw material, ultrasound 60min in methanol solution is added in；Wherein whisker carbon nanotubes, aluminum nitrate and methanol molar ratio are 1:1:
182, obtain whisker carbon nanotube suspension；The suspension is imported in hydrothermal reaction kettle, wherein suspension volume accounts for reaction kettle
Molten product 40%.It places into reacting furnace and heats, be warming up to 120 DEG C with 3 DEG C/min, keep the temperature 1h, then 150 DEG C are warming up to 1 DEG C/min
Afterwards, 12h is kept the temperature；It is put into after filtering low temperature drying after being cooled to room temperature with 10 DEG C/min in corundum crucible with 700 DEG C of high-temperature roastings 3
Hour, the whisker carbon nano-tube material of coating alumina is obtained, the process is whole to import argon gas protection.
Mass fraction is put into low power ultrasound in methanol for the whisker carbon nanotubes of 4% coating alumina of Al alloy powder
Concussion obtains the whisker carbon nanotube suspension of coating alumina, time control 20min.By 2024 aluminium alloys of corresponding mass
Powder imports suspension and obtains mixing batch mixing and in 100 DEG C of vacuum dryings.Gained mixed-powder is put into 60MPa cold pressings pressure in mold
Block is made, gained prefabricated section is put into corresponding mold groove, and the mold is heated to 480 DEG C with the 5 DEG C/min rates of heat addition.With 5
DEG C/min continue to heat and control its solid rate in 70% or so it is rear carry out die-forging forming processing, with 90mm/s pressure head rates, pressurize
Time is 5min postcoolings to room temperature, obtains the aluminum matrix composite drip molding of the whisker carbon nanotubes of coating alumina/2024.
Claims (2)
1. a kind of preparation method of the whisker carbon nanotube enhanced aluminium-based composite material of coating alumina, it is characterized in that including following
Step：
（1）By whisker carbon nanotubes in the pure salpeter solution pre-dispersed 6 ~ 8h of ultrasound, temperature is 60 ~ 80 DEG C, after being cooled to room temperature, is used
Deionized water is cleaned, and is centrifuged to neutrality, is then dried in vacuum drying chamber, spare；
（2）By aluminum nitrate and through step（1）The whisker carbon nanotubes of pretreatment be added in methanol solution ultrasound 40~
60min obtains whisker carbon nanotube suspension, wherein whisker carbon nanotubes and nitric acid al mole ratio 1:0.4~1:1；
（3）Through step（2）Whisker carbon nanotube suspension import hydrothermal reaction kettle in, wherein suspension volume accounts for reaction kettle
Volume 25%~40%；It places into reacting furnace and heats, be warming up to 100~120 DEG C with 1~5 DEG C/min, keep the temperature 1~2h, then with 1
After~3 DEG C/min is warming up to 150 DEG C, 8~12h is kept the temperature；Low temperature drying is filtered after being cooled to room temperature with 5 ~ 10 DEG C/min；
（4）Through step（3）Gained mixing material is put into corundum crucible, and when 480 ~ 700 DEG C of high-temperature roastings 3 are small, whole process imports
Argon gas is protected, and obtains the whisker carbon nano-tube material of coating alumina；
（5）The whisker carbon nano-tube material of coating alumina is put into low power ultrasonic vibration≤30min in methanol, obtains coating oxygen
Change the whisker carbon nanotube suspension of aluminium；
（6）Al alloy powder is imported in suspension and is stirred, obtains mixture, and in 50 ~ 100 DEG C of vacuum dryings；Wherein coat oxygen
The whisker carbon nanotubes for changing aluminium accounts for the 1% ~ 4% of aluminium alloy gross mass；
（7）Step（6）Obtained mixture is put into ball milling crucible and carries out ball milling, and being passed through argon gas in the mechanical milling process is protected
Shield；
（8）Step（7）Gained mixed-powder is put into 60 ~ 150MPa in mold and is pressed into prefabricated section；
（9）Step（8）Gained prefabricated section is put into corresponding mold groove, and the mold is heated with 5 ~ 10 DEG C/min rates of heat addition
To 10 ~ 20 DEG C of subsolidus, 1 ~ 5 DEG C/min continues to heat and controls its solid rate in 70 ~ 90% scopes；
（10）Step（9）Gained moulding mixture carries out die-forging forming, and pressure head is controlled after 20 ~ 130mm/s rates, 5 ~ 10min of pressurize
It is cooled to room temperature to obtain the whisker carbon nanotube enhanced aluminium-based composite material drip molding of coating alumina.
2. preparation method according to claim 1, it is characterized in that step（3）The hydrothermal reaction kettle liner is polytetrafluoro
Ethylene.
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| CN110669956A (en) * | 2019-11-21 | 2020-01-10 | 吉林大学 | Preparation method of carbon nano tube reinforced aluminum-based composite material with surface coated with aluminum oxide |
| CN111349835B (en) * | 2020-05-12 | 2021-09-28 | 西南石油大学 | Alloy, preparation method and application thereof |
| CN113088744B (en) * | 2021-02-20 | 2022-03-22 | 南昌大学 | Preparation method of modified carbon nanotube reinforced aluminum alloy semi-solid slurry |
| CN113088745B (en) * | 2021-02-20 | 2022-05-20 | 南昌大学 | Preparation method of zirconium oxide coated carbon nanotube reinforced aluminum matrix composite |
| CN113444906B (en) * | 2021-06-10 | 2023-06-16 | 湘潭大学 | Method for preparing carbon nano tube reinforced light aluminum-based alloy |
| CN115747591B (en) * | 2022-11-28 | 2024-02-13 | 凤阳爱尔思轻合金精密成型有限公司 | High-toughness aluminum alloy material and preparation process thereof |
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